CN113182062A - Method for flotation of flake graphite ore - Google Patents

Method for flotation of flake graphite ore Download PDF

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Publication number
CN113182062A
CN113182062A CN202110544914.4A CN202110544914A CN113182062A CN 113182062 A CN113182062 A CN 113182062A CN 202110544914 A CN202110544914 A CN 202110544914A CN 113182062 A CN113182062 A CN 113182062A
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China
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flotation
concentrate
ore
graphite
concentration
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陶东平
马芳源
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Shandong University of Technology
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Shandong University of Technology
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Priority to CN202110544914.4A priority Critical patent/CN113182062A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/08—Separating or sorting of material, associated with crushing or disintegrating
    • 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
    • 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
    • B03D1/14—Flotation machines
    • 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
    • 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
    • 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
    • B03D2201/04—Frothers
    • 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
    • B03D2201/06—Depressants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00—Specified materials treated by the flotation agents; specified applications
    • B03D2203/02—Ores

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Food Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biotechnology (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention provides a method for flotation of flake graphite ore, and belongs to the technical field of graphite ore dressing. The high-pressure roller milling is adopted, so that the protection of the scale is facilitated, and the graphite dissociation is promoted; the stirring grinding is adopted to facilitate the slippage of the symbiotic interface of graphite and gangue; the flotation effect can be improved by limiting the flotation column during the concentration operation. In the invention, the reduction of the number of grinding sections depends on the combination of the high-pressure roller mill and the stirring mill, the reduction of the length of the flotation process depends on the flotation column selected in the concentration, and the graphite concentrate with higher grade can be obtained only by repeating the steps for 1-3 times. The results of the embodiment show that only one section of high-pressure roller mill, two sections of stirring mills and three sections of flotation are needed by adopting the flotation method provided by the invention, compared with the traditional flotation process, the recovery rate of the graphite concentrate is improved by 10-15% by the method provided by the invention, and the grade of the graphite concentrate is improved by 0-0.2%.

Description

Method for flotation of flake graphite ore
Technical Field
The invention relates to the technical field of graphite ore dressing, in particular to a short-process flake graphite ore flotation method.
Background
Graphite is an emerging strategic resource and plays a certain decisive role in advancing national economy and scientific research, so that the graphite is widely called as 'black gold', and the graphite resource is an indispensable important material resource in the 21 st century. China has abundant graphite reserves of about 5500 ten thousand tons, and annual output and export are in the forefront of the world. China mainly focuses on medium and small-sized enterprises, and in view of overlong production process, high cost of rough machining investment and low economic benefit brought by rough machining products, and still has many problems such as laggard selection process, weak technological innovation capability, environmental destruction, resource waste and the like, so that the overall utilization of graphite resources in China still lags behind developed countries.
The continuous exploitation of graphite resources causes the gradual reduction of large-scale and easily-dissociated graphite deposits, and accordingly, low-grade and difficultly-treated graphite becomes a main choice for recycling graphite in China. The fine flake graphite will be the main strategic resource currently exploited and utilized. However, the grade of the fine flake graphite is low, the selectivity is low, and in order to obtain graphite concentrate with the fixed carbon content higher than 94%, a longer grinding and selecting process is needed, generally seven-grinding eight-grinding selection is needed, and the longer grinding and even nine-grinding ten-grinding selection is needed. The overlong grinding and separation process can obviously increase the cost of ore separation and the energy consumption of products, and can simultaneously cause more middlings, and the instability of flotation indexes is easily caused in the process of returning the excessive middlings, so that the efficiency of ore separation is reduced. Therefore, it is highly desirable to provide a method for efficiently and short-process flotation of flake graphite ore.
Disclosure of Invention
The invention aims to provide a high-efficiency short-flow scale graphite ore flotation method.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for flotation of scale graphite ore, which comprises the following steps:
(1) carrying out high-pressure roller milling on the flake graphite raw ore to obtain crushed raw ore; mixing the crushed raw ore with a collecting agent, a foaming agent, a pH control agent and an inhibitor, and performing roughing operation to obtain roughed tailings and roughed concentrate;
(2) stirring and grinding the rough concentration obtained in the step (1), and then carrying out concentration operation to obtain concentrated tailings and concentrated concentrate;
(3) repeating the operation of the concentration operation after the stirring and grinding in the step (2) on the concentration concentrate obtained in the step (2) to obtain final concentrate and final tailings; the repetition frequency is 1-3 times;
and (3) the flotation column used in the concentration operation in the step (2) and the step (3) is a static micro-bubble cyclone flotation column.
Preferably, the mass percentage of the particle size of-0.074 mm in the crushed raw ore in the step (1) is 60-70%.
Preferably, on the basis of the mass of the crushed raw ore, the using amount of the collecting agent in the step (1) is 300-400 g/t, the using amount of the foaming agent is 300-400 g/t, and the using amount of the inhibitor is 1200-1500 g/t; the pH value of the ore pulp in the roughing operation process is controlled to be 10-11, and the mass concentration of the ore pulp is 5-10%.
Preferably, the mass percentage of the product with the particle size of-0.074 mm obtained by stirring and grinding in the step (2) is 80-85%.
Preferably, the mass percentage of the product with the particle size of-0.074 mm obtained by stirring and grinding in the step (3) is 74-78%.
Preferably, the particle size of the ore grinding medium used in the stirring mill in the step (2) and the step (3) is 2-5 mm.
Preferably, during the concentration operation in the step (2), the pH value of the ore pulp is controlled to be 10-11; adding foaming agent in the fine selection process; the addition amount of the foaming agent is 500-600 g/t on the basis of the mass of the crushed raw ore.
Preferably, in the concentration process of the step (3), the pH value of the ore pulp is controlled to be 10-11; adding foaming agent in the fine selection process; the addition amount of the foaming agent is 800-1000 g/t on the basis of the mass of the crushed raw ore.
Preferably, the feeding speed of the flotation column in the roughing operation in the step (1) and the feeding speed of the flotation column in the concentrating operation in the step (2) are 0.6-0.8L/min, and the feeding speed of the flotation column in the concentrating operation in the step (3) is 0.4-0.5L/min.
Preferably, the aeration amount in the roughing operation in the step (1), the refining operation in the step (2) and the refining operation in the step (3) is 0.8-1.2L/min independently, the thickness of the foam layer is 25-30 cm independently, and the flow rate of flushing water is 0.3-0.5L/min independently.
The invention provides a method for flotation of scale graphite ore, which comprises the following steps: (1) carrying out high-pressure roller milling on the flake graphite raw ore to obtain crushed raw ore; mixing the crushed raw ore with a collecting agent, a foaming agent, a pH control agent and an inhibitor, and performing roughing operation to obtain roughed tailings and roughed concentrate; (2) stirring and grinding the rough concentration obtained in the step (1), and then carrying out concentration operation to obtain concentrated tailings and concentrated concentrate; (3) repeating the operation of the concentration operation after the stirring and grinding in the step (2) on the concentration concentrate obtained in the step (2) to obtain final concentrate and final tailings; the repetition frequency is 1-3 times; and (3) the flotation column used in the concentration operation in the step (2) and the step (3) is a static micro-bubble cyclone flotation column. According to the invention, the high-pressure roller mill is adopted to selectively crush graphite ores, so that the intergrowth interface of graphite flakes and gangue is promoted to crack, the gangue is exposed, the protection of the flakes is facilitated, and the graphite dissociation is promoted; the stirring grinding is adopted to facilitate the slippage of the symbiotic interface of graphite and gangue; the invention can improve the flotation effect by limiting the flotation column during the concentration operation. In the invention, the reduction of the number of grinding sections depends on the combination of the high-pressure roller mill and the stirring mill, the reduction of the length of the flotation process depends on the flotation device selected in the concentration, and the higher-grade graphite concentrate can be obtained only by repeating the steps for 1-3 times. The results of the embodiment show that by adopting the flotation method provided by the invention, the fine graphite with the particle size of 2-3 mu m can be effectively recycled only by one section of high-pressure roller mill, two sections of stirring mill and three sections of flotation, and compared with the conventional flotation process, the lower limit of the sorting particle size is 6 mu m, the method provided by the invention obviously improves the recycling effect of the fine graphite; compared with the traditional flotation process, the method provided by the invention has the advantages that the recovery rate of the graphite concentrate is improved by 10-15%, and the grade of the graphite concentrate is improved by 0-0.2%.
Drawings
FIG. 1 is a schematic diagram of a flake graphite ore flotation method provided by the present invention;
FIG. 2 is a flow diagram of a conventional flotation process used in comparative example 1 of the present invention;
figure 3 is a graph of the particle size distribution of the final concentrate from the flotation processes of example 1 and comparative example 1 of the present invention.
Detailed Description
The invention provides a method for flotation of scale graphite ore, which comprises the following steps:
(1) carrying out high-pressure roller milling on the flake graphite raw ore to obtain crushed raw ore; mixing the crushed raw ore with a collecting agent, a foaming agent, a pH control agent and an inhibitor, and performing roughing operation to obtain roughed tailings and roughed concentrate;
(2) stirring and grinding the rough concentration obtained in the step (1), and then carrying out concentration operation to obtain concentrated tailings and concentrated concentrate;
(3) repeating the operation of the concentration operation after the stirring and grinding in the step (2) on the concentration concentrate obtained in the step (2) to obtain final concentrate and final tailings; the repetition frequency is 1-3 times;
and (3) the flotation column used in the concentration operation in the step (2) and the step (3) is a static micro-bubble cyclone flotation column.
The method comprises the steps of carrying out high-pressure roller grinding on flake graphite raw ore to obtain crushed raw ore; and mixing the crushed raw ore with a collecting agent, a foaming agent, a pH control agent and an inhibitor, and performing roughing operation to obtain roughed tailings and roughed concentrate.
The source of the flake graphite raw ore is not particularly limited, and the flake graphite raw ore can be obtained by a person skilled in the art.
In the present invention, the high pressure roller mill is preferably a high pressure roller mill. In the invention, the high-pressure roller mill can selectively crush flake graphite raw ores, promote the intergrowth interface of graphite flakes and gangue to crack, expose the gangue, be beneficial to the protection of the flakes and promote the dissociation of the graphite. The type of the high-pressure roller mill is not particularly limited, and a high-pressure roller mill known by a person skilled in the art can be adopted.
In the invention, the mass percentage of the particle size of-0.074 mm in the crushed raw ore is preferably 60-70%, more preferably 65-70%. In the invention, when the mass percentage of the particle size of the crushed raw ore is-0.074 mm in the range, the raw flake graphite can be fully dissociated, the poor dissociation effect caused by too coarse fineness of the raw flake graphite can be prevented, the grade of graphite can be lower, the mineralization effect in the flotation process caused by too fine raw flake graphite can be prevented from being deteriorated, the recovery rate can be lower, and the recovery rate of graphite concentrate can be further improved.
The operating parameters of the high-pressure roller mill are not particularly limited, and the mass percentage of the particle size of-0.074 mm in the crushed raw ore can be preferably 60-70%. In the present invention, the parameters of the high pressure roller mill preferably include: the feeding granularity is preferably 25-30 mm, the working pressure is preferably 5-6 Mpa, the roller surface rotating speed is 18-20 r/min, and the distance between rollers is 5-6 mm.
After the crushed raw ore is obtained, the crushed raw ore is mixed with a collecting agent, a foaming agent, a pH control agent and an inhibitor, and roughing operation is performed to obtain roughed tailings and roughed concentrate.
In the invention, the use amount of the collecting agent is preferably 300-400 g/t, and more preferably 350-400 g/t based on the mass of the crushed raw ore. In the invention, the collecting agent plays a role in sorting the scale graphite minerals. In the invention, when the using amount of the collecting agent is in the range, the poor intergrowth of some graphite collected when the using amount of the collecting agent is too high can be prevented from influencing the grade, the condition that the foam is unstable and influences the recovery rate when the using amount of the collecting agent is too low can be prevented, and the recovery rate of the concentrate can be further improved. The invention is not particularly limited in the kind of the collector, and a collector well known to those skilled in the art may be used. In the present invention, the collector preferably comprises kerosene or diesel oil.
In the invention, the amount of the foaming agent is preferably 300 to 400g/t, and more preferably 350 to 400g/t, based on the mass of the crushed raw ore. In the invention, the foaming agent is beneficial to the formation of bubbles in the flotation pulp, and when the consumption of the foaming agent is in the range, the situation that the bubble load capacity is too strong due to too high consumption of the foaming agent and the grade is reduced due to poor intergrowth or gangue particle inclusion is serious can be prevented, the situation that the recovery rate is reduced due to too low foaming load capacity due to too low consumption of the foaming agent can be prevented, and the recovery rate and the grade of graphite concentrate can be further improved. The type of the blowing agent is not particularly limited in the present invention, and any blowing agent known to those skilled in the art may be used. In the present invention, the foaming agent preferably comprises No. two oil, sec-octanol or industrial waste fusel.
In the invention, the pH control agent can control the pH value in the system, and the pH value of the ore pulp in the roughing operation process is preferably controlled to be 10-11. In the invention, when the pH value in the ore pulp in the roughing operation process is in the range, the surface potential of the gangue minerals can be adjusted, which is beneficial to the recovery rate of graphite concentrate. The kind of the pH control agent is not particularly limited in the present invention, and a pH control agent known to those skilled in the art may be used. In the invention, when the gangue in the raw ore of the graphite of the phosphorite contains pyrite, the pH control agent is preferably quicklime; when the gangue in the raw graphite phosphate ore does not contain pyrite, the pH control agent is preferably sodium carbonate.
In the invention, the dosage of the inhibitor is preferably 1200-1500 g/t, more preferably 1300-1400 g/t based on the mass of the crushed raw ore. In the invention, the inhibitor can promote the improvement of the recovery rate of the graphite concentrate. In the present invention, when the amount of the inhibitor is within the above range, it is possible to prevent the reduction in the recovery rate due to excessive inhibition of the intergrowth of graphite by an excessively large amount of the inhibitor, and also possible to prevent the reduction in the grade due to the incomplete inhibition of the poor intergrowth due to an excessively low amount of the inhibitor, thereby improving the recovery rate and grade of the graphite concentrate. The type of the inhibitor is not particularly limited in the present invention, and any inhibitor known to those skilled in the art may be used. In the present invention, the inhibitor is preferably sodium hexametaphosphate.
In the invention, the mass concentration of the ore pulp is preferably 5-10%, and more preferably 6-8%. In the invention, when the mass concentration of the ore pulp is in the range, the phenomenon that the concentration of the ore pulp is too high, which can cause the collapse of a foam layer due to too low air bubble loading capacity can be prevented.
The operation mode of mixing the crushed raw ore with the collecting agent, the foaming agent, the pH control agent and the inhibitor is not particularly limited, and the mixing mode known by the person skilled in the art can be adopted.
In the invention, the adding amount of the collecting agent, the foaming agent, the pH control agent and the inhibitor is based on the mass of the crushed raw ore, but in order to compare the difference between the conventional flotation process and the process of the invention, the amounts of the collecting agent, the foaming agent, the pH control agent and the inhibitor consumed in the production of 1t total concentrate are generally compared, because in the actual production process, because the conventional flotation process has too many ore grinding stages and the process is complex, the dosage of the agent in each stage of the flotation operation is in a dynamic change, and the accurate dosage of the agent cannot be collected for each flotation operation. Thus, the amounts of collector, frother, pH control agent and depressant added are based on 1t total concentrate produced when compared to the amounts consumed for conventional flotation processes and the process of the present invention. In the present invention, when the collector, the frothing agent, the pH controlling agent and the inhibitor are in the above ranges in the steps (1) to (3), the collector consumed in terms of producing 1t of total concentrate is preferably (6 to 9) kg/t, more preferably (8 to 9) kg/t; the foaming agent is preferably (5-8) kg/t, and more preferably (6-7) kg/t; the pH control agent is preferably (220-250) kg/t, more preferably (240-250) kg/t; the inhibitor is preferably (10-15) kg/t, more preferably (12-13) kg/t.
After the mixing is finished, the system obtained by mixing is subjected to roughing operation to obtain roughing tailings and roughing concentrate.
The flotation column used in the roughing operation is not particularly limited in the present invention, and a flotation column known to those skilled in the art may be used. In the present invention, the flotation column used in the rougher flotation is preferably a conventional bubble generator flotation column. In the invention, the graphite ore obtained after the high-pressure roller milling has a relatively large particle size, and a good mineralization effect can be achieved by adopting a conventional bubble generator.
In the invention, the feeding speed of the flotation column during the roughing operation is preferably 0.6-0.8L/min, and more preferably 0.7-0.8L/min. In the invention, when the ore feeding speed of the flotation column is in the range, the recovery rate and the grade of the graphite concentrate are favorably improved.
In the invention, the aeration amount during the roughing operation is preferably 0.8-1.2L/min, and more preferably 1.0-1.2L/min. In the invention, when the aeration quantity in the roughing operation is in the range, the recovery rate and the grade of the graphite concentrate are favorably improved.
In the present invention, the thickness of the foam layer in the roughing operation is preferably 25 to 30cm, and more preferably 25 to 28 cm. In the present invention, when the thickness of the froth layer in the roughing operation is in the above range, it is advantageous to improve the recovery rate and grade of the graphite concentrate.
In the invention, the flow rate of the washing water in the roughing operation is preferably 0.3-0.5L/min, and more preferably 0.4-0.5L/min. In the present invention, when the flow rate of the washing water in the roughing operation is in the above range, it is advantageous to improve the recovery rate and grade of the graphite concentrate.
After the roughing concentrate is obtained, the roughing concentrate is stirred and ground, and then the concentration operation is carried out, so that the concentration tailings and the concentration concentrate are obtained.
In the invention, the mass percentage of the product with the particle size of-0.074 mm obtained by stirring and grinding is preferably 80-85%, and more preferably 82-85%. In the invention, when the mass percentage of the particle size of-0.074 mm in the product obtained by the stirring mill is in the above range, the product obtained by the stirring mill can be prevented from having poor dissociation effect due to too coarse particle size, so that the grade of graphite is relatively low, and the mineralization effect in the flotation process is deteriorated due to too small particle size, so that the recovery rate is relatively low, thereby further improving the grade and recovery rate of recovered graphite concentrate.
In the invention, the stirring mill grinding mainly takes the shearing action of a medium as a main part, is beneficial to promoting the slippage of a symbiotic interface of graphite and gangue, has small damage degree to scales and good dissociation effect, and reduces the number of grinding sections. The stirring and grinding device is not particularly limited, and the particle size of the roughed concentrate can be ground to the range. In the present invention, the stirring mill is preferably a stirring mill. The stirring and grinding device is not particularly limited, and the particle size of the roughed concentrate can be ground to the range.
In the invention, the particle size of the ore grinding medium used for the stirring mill is preferably 2-5 mm, and more preferably 3-4 mm. In the invention, the scale is seriously damaged due to overlarge kinetic energy of the medium in the ore grinding process caused by overlarge medium particle size, the particle size is thinned, the recovery difficulty is increased, and the recovery rate is reduced. In the present invention, when the particle size of the medium is within the above range, it is advantageous to further control the recovery rate of the concentrate.
After the stirring mill is finished, the invention carries out concentration operation on the product obtained after the stirring mill to obtain concentration tailings and concentration concentrate.
In the invention, the flotation column in the concentration operation is a static micro-bubble rotational flow flotation column. In the invention, the bubbles generated by the static micro-bubble rotational flow flotation column are micro bubbles or nano bubbles, which is beneficial to mineralizing fine particle graphite; in addition, the mode of generating bubbles by the static microbubble cyclone flotation column is a hydrodynamic cavitation principle, the bubbles nucleate and separate out on the surface of graphite, the hydrophobicity of the surface of the graphite is increased, the flotation selectivity is good, the wetting film on the surface of the graphite is favorably broken, the first separation can be considered in the cyclone area of the flotation column, the second separation can be considered in the static flow area, and the improvement of the grade of graphite concentrate is favorably realized; in addition, the circulating device of the static microbubble spiral flow flotation column has a secondary mineralization effect on middlings, can be considered as scavenging operation, and is beneficial to improving the recovery rate. Therefore, in the invention, when the flotation column in the concentration operation adopts a static micro-bubble cyclone flotation column, the recovery rate and the grade of the graphite concentrate can be ensured. The method of operation of the concentration operation in the present invention is not particularly limited, and the method of operation known to those skilled in the art may be used.
In the present invention, it is preferable to supplement the frother during the concentration operation. In the present invention, the addition amount of the foaming agent is preferably 500 to 600g/t, more preferably 550 to 600g/t, based on the mass of the crushed raw ore. In the invention, when the addition amount of the foaming agent is in the range, the recovery rate and the grade of the concentrate can be further improved by controlling the using amount of the foaming agent in the concentration operation. The type of the additional blowing agent is not particularly limited in the present invention, and any blowing agent known to those skilled in the art may be used. In the present invention, the foaming agent preferably comprises No. two oil, sec-octanol or industrial waste fusel.
In the invention, the pH value of the ore pulp is preferably controlled between 10 and 11 in the concentration operation process. In the present invention, the function of controlling the pH value in the system during the concentration operation is the same as that during the roughing operation, and the detailed description thereof is omitted.
In the invention, the ore feeding speed of the flotation column during the concentration operation is preferably 0.6-0.8L/min, and more preferably 0.6-0.8L/min. In the invention, when the ore feeding speed of the flotation column is in the range, the recovery rate and the grade of the graphite concentrate are favorably improved.
In the invention, the aeration amount in the concentration operation is preferably 0.8-1.2L/min, and more preferably 1.0-1.2L/min. In the invention, when the aeration quantity in the concentration operation is in the range, the recovery rate and the grade of the graphite concentrate are favorably improved.
In the present invention, the thickness of the foam layer in the concentration operation is preferably 25 to 30cm, and more preferably 25 to 28 cm. In the invention, when the thickness of the foam layer in the concentration operation is in the range, the recovery rate and the grade of the graphite concentrate can be improved.
In the present invention, the flow rate of the washing water in the concentration operation is preferably 0.3 to 0.5L/min, and more preferably 0.4 to 0.5L/min. In the invention, when the flow of the washing water in the concentration operation is in the range, the recovery rate and the grade of the graphite concentrate can be improved.
After the obtained concentrated concentrate is obtained, the operation of the concentration operation after the stirring and grinding in the technical scheme is repeated on the concentrated concentrate to obtain the final concentrate and the final tailings.
In the invention, the mass percentage of the product with the particle size of-0.074 mm obtained after the concentration concentrate is stirred and ground is preferably 74-78%, and more preferably 75-77%. In the invention, when the mass percentage of the product with the particle size of-0.074 mm in the product obtained by repeatedly stirring and grinding the concentrated concentrate in the steps is in the range, the recovery rate of the graphite concentrate can be improved.
In the invention, the number of times of the step of repeated stirring and grinding of the concentrated concentrate is 1-3 times, and preferably 1 time. In the invention, the adopted raw material is flake graphite raw ore, the refined concentrate is repeatedly stirred and ground for 1-3 times by adopting the method provided by the invention, so that the mass percentage of the product with the particle size of-0.074 mm in the refined concentrate obtained after the repeated stirring and grinding is preferably 74-78%, and the graphite concentrate with high recovery rate and high grade can be obtained.
In the invention, the flotation column used in the concentration operation after the concentration concentrate is repeatedly stirred and ground is a static micro-bubble rotational flow flotation column. In the invention, when the device adopted by the flotation column in the concentration operation after the repeated stirring and grinding of the concentrated concentrate is a static microbubble cyclone flotation column, the recovery rate and the grade of the graphite concentrate can be ensured. The method of operation of the concentration operation in the present invention is not particularly limited, and the method of operation known to those skilled in the art may be used.
In the invention, the foaming agent is preferably supplemented in the concentration operation process after the concentration concentrate is repeatedly stirred and ground. In the present invention, the addition amount of the foaming agent is preferably 800 to 1000g/t, and more preferably 900 to 1000g/t, based on the mass of the crushed raw ore. In the invention, when the amount of the foaming agent added in the concentration operation process after the concentration concentrate is repeatedly stirred and ground is in the range, the amount of the foaming agent in the concentration operation can be controlled, so that the recovery rate and the grade of the concentrate can be further improved. The type of the additional blowing agent is not particularly limited in the present invention, and any blowing agent known to those skilled in the art may be used. In the present invention, the foaming agent preferably comprises No. two oil, sec-octanol or industrial waste fusel.
In the invention, the pH value of the system during concentration operation after repeated stirring and grinding of the concentrated concentrate is preferably controlled to be 10-11. In the invention, the function of controlling the pH value in the system during the concentration operation after the concentration concentrate is repeatedly stirred and ground is the same as that during the rough concentration operation and the concentration operation, and the detailed description is omitted here.
In the invention, the ore feeding speed of the flotation column during the concentration operation after the repeated stirring and grinding of the concentrated concentrate is preferably 0.4-0.5L/min. In the invention, when the ore feeding speed of the flotation column is in the range, the recovery rate and the grade of the graphite concentrate are favorably improved.
In the invention, the aeration quantity of the selected concentrate in the selecting operation after repeated stirring and grinding is preferably 0.8-1.2L/min, and more preferably 1.0-1.2L/min. In the invention, when the aeration quantity in the concentration operation after the concentration concentrate is repeatedly stirred and ground is in the range, the recovery rate and the grade of the graphite concentrate are favorably improved.
In the invention, the thickness of the foam layer of the selected concentrate in the selecting operation after repeated stirring and grinding is preferably 25-30 cm, and more preferably 25-28 cm. In the invention, when the thickness of the foam layer in the concentration operation after the concentration concentrate is repeatedly stirred and ground is in the range, the recovery rate and the grade of the graphite concentrate are favorably improved.
In the invention, the flow of flushing water in the concentration operation after the repeated stirring and grinding of the concentrated concentrate is preferably 0.3-0.5L/min, and more preferably 0.4-0.5L/min. In the invention, when the flow of flushing water in the concentration operation after the concentration concentrate is repeatedly stirred and ground is in the range, the recovery rate and the grade of the graphite concentrate are favorably improved.
The schematic diagram of the flake graphite ore flotation method provided by the invention is preferably shown in figure 1. As can be seen from fig. 1, after being subjected to high-pressure roll milling, the flake graphite raw ore is mixed with a collecting agent, a foaming agent, a pH control agent and an inhibitor, and is subjected to roughing operation to obtain roughed tailings and roughed concentrate; stirring and grinding the obtained rough concentration, adding a foaming agent, and then carrying out fine concentration operation to obtain fine concentration tailings and fine concentration concentrate; and stirring and grinding the obtained concentrated concentrate, adding a foaming agent, then carrying out concentration operation to obtain final concentrate and final tailings, and then recovering the roughed tailings, the concentrated tailings and the final tailings into total tailings.
According to the invention, the high-pressure roller mill is adopted to selectively crush graphite ores, so that the intergrowth interface of graphite flakes and gangue is promoted to crack, the gangue is exposed, the protection of the flakes is facilitated, and the graphite dissociation is promoted; the stirring grinding is adopted to facilitate the slippage of the symbiotic interface of graphite and gangue; the flotation effect can be improved by setting the device during the selection operation. In the invention, the reduction of the number of grinding sections depends on the combination of the high-pressure roller mill and the stirring mill, the reduction of the length of the flotation process depends on the flotation device selected in the concentration, and the higher-grade graphite concentrate can be obtained only by repeating the steps for 1-3 times.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Raw materials: the content of fixed carbon in the fine flake graphite in the North-Notyoeli prefecture of Heilongjiang is 11.15%, and the main gangue minerals are quartz, muscovite and pyrite.
(1) Carrying out high-pressure roller milling on the fine flake graphite in the Luo Bei county of the Heilongjiang province by using a high-pressure roller mill to obtain 65 mass percent crushed raw ore with the particle size of-0.074 mm. Mixing the crushed raw ore with a collecting agent, a foaming agent, a pH control agent and an inhibitor, and performing roughing operation to obtain roughed tailings and roughed concentrate; the bubble generator adopted by the flotation column in the roughing operation is a conventional bubble generator;
wherein, diesel oil is used as a collector, and the using amount of the collector is 400 g/t; taking industrial fusel as a foaming agent, wherein the dosage of the foaming agent is 300 g/t; quicklime is used as a pH control agent to ensure that the pH value in the system is 10; sodium hexametaphosphate is taken as an inhibitor, and the dosage of the inhibitor is 1500 g/t. (the amounts of collector, frother, pH control agent and inhibitor are all relative to the mass of the crushed raw ore)
Conditions in roughing: the aeration rate is 0.9L/min, the ore feeding speed is 0.8L/min, the thickness of the foam layer is 30cm, and the flushing water speed is 0.4L/min.
(2) Stirring and grinding the roughed concentrate obtained in the step (1) to obtain a product with the fineness of 0.074mm and the mass percentage of 81.5%, and then carrying out concentration operation on the obtained product to obtain concentrated tailings and concentrated concentrate;
500g/t is supplemented with the amount of the foaming agent, and the bubble generator adopted by the flotation column in the concentration operation is a nano bubble generator;
the parameters of the fine selection operation are as follows: the aeration quantity is 1L/min, the ore feeding speed is 0.8L/min, the thickness of the foam layer is 30cm, the flushing water speed is 0.5L/min, and the pH value is 10.
(3) Repeating the stirring and grinding in the step (2) on the concentrated concentrate obtained in the step (2) to obtain a product with the fineness of 0.074mm and the mass percentage of 75.1%, and then carrying out concentration operation on the obtained product to obtain final concentrate and final tailings; the number of repetitions is 1;
800g/t is added in the amount of the foaming agent, and the bubble generator adopted by the flotation column in the concentration operation is a nano bubble generator;
the parameters of the fine selection operation are as follows: the aeration quantity is 1L/min, the ore feeding speed is 0.5L/min, the thickness of the foam layer is 30cm, the flushing water speed is 0.5L/min, and the pH value is 10.
(4) And (4) calculating the medicament dosage of the conventional flotation process according to the 1t total concentrate obtained in the steps (1) to (3), wherein the medicament dosage of a collecting agent is 3.48kg/t concentrate, the foaming agent dosage is 5.67kg/t concentrate, the pH regulator dosage is 250kg/t concentrate, and the inhibitor dosage is 13 kg/t.
The performance and specific experimental parameters of the product obtained by performing flotation on the fine flake graphite in the north of norway prefecture of black dragon river by the flotation method in this example are shown in table 1.
The room temperature particle size of the final concentrate prepared in this example was analyzed by a laser particle size analyzer to obtain a particle size distribution diagram as shown in fig. 3.
Comparative example 1
This comparative example is a conventional flotation process, and the flow diagram is shown in figure 2. As can be seen from fig. 2, the method of the conventional flotation process includes:
(1) performing ball milling on fine flake graphite in the North-Notyoeli county of Heilongjiang province by adopting a ball milling method to obtain crushed raw ore with the particle size of-0.074 mm and the mass percent of 80%, mixing the crushed raw ore with a collecting agent, a foaming agent, a pH control agent and an inhibitor, and performing roughing operation to obtain tailings 1 and roughed concentrate 1; the flotation equipment during the roughing operation adopts a mechanical stirring type flotation machine;
wherein, diesel oil is used as a collector, and the using amount of the collector is 800 g/t; the industrial fusel is used as a foaming agent, the dosage of the foaming agent is 400g/t, the quicklime is used as a pH control agent, and the pH is 10.
(2) And (3) performing rod grinding for 1 time and flotation open-circuit flow for 1 time on the concentrate in the step (1) to obtain flotation concentrate and tailings 2.
(3) And (3) performing sand grinding and flotation open-circuit flow 1 time on the roughed concentrate obtained in the step (2) to obtain tailings 3 and flotation concentrate.
(4) And (3) repeating the step (2), and performing 7 times of sanding and 7 times of flotation open-circuit processes on the flotation concentrate obtained in the step (2) to obtain 4-10 tailings and total concentrate. Wherein, the tailings are treated into a total tailing by 1-10 unification.
(5) And (4) calculating the medicament dosage of the conventional flotation process according to the 1t total concentrate produced in the steps (1) to (4), wherein the medicament dosage is 9kg/t concentrate, the foaming agent dosage is 5.8kg/t concentrate, and the pH regulator dosage is 267kg/t concentrate.
The performance and specific experimental parameters of the product obtained by performing flotation on the fine flake graphite in the northwest of black dragon river by using the flotation method of the comparative example are shown in table 1.
The room temperature particle size of the final concentrate prepared in this example was analyzed by a laser particle size analyzer to obtain a particle size distribution diagram as shown in fig. 3.
Table 1: agent/equipment/flotation conditions/product index for flotation processes of example 1 and comparative example 1
Figure BDA0003073245830000121
Figure BDA0003073245830000131
As can be seen from table 1, the recovery of graphite concentrate obtained by the alternative flotation method of the present application is improved by about 14.73%, the concentrate grade is improved by about 0.2%, and the concentrate yield is improved by 1.71% as compared to the conventional flotation process. Although the yield of the concentrate product of the new flotation process, namely the ore product of the 100 meshes, is slightly lower than that of the conventional flotation process, the proportion of the yield of the concentrate of the new flotation process, namely the ore product of the 100 meshes, in the raw ore is higher than that of the conventional flotation process by 0.13%, and the yield of large-scale graphite is obviously improved by the new flotation process.
The lower limit of the final concentrate granularity recovered by the flake graphite ore flotation method provided by the invention is 2 microns, and the minimum granularity recovered by the conventional flotation method is 6 microns, so that the recovery effect of the flotation process provided by the invention on the ultrafine particle graphite is far higher than that of the conventional flotation method. In addition, the rough flotation granularity of the flotation process provided by the invention is only 65 percent of-0.074 mm by mass percent, while the conventional flotation granularity is 80 percent. The flotation process provided by the invention reduces the number of the flotation stages and the number of the grinding stages to three stages, and reduces the grinding and flotation operations of seven stages compared with the conventional flotation. In terms of the amount of flotation agents, the amount of collecting agent saved by the new flotation process for producing 1t concentrate is at least 1/2 of the conventional flotation process, the amount of pH regulator is saved by 17kg/t concentrate, and the amounts of foaming agents used in the two processes are equivalent. Unlike conventional flotation processes, the new flotation process requires 13kg of depressants to be added to produce 1 ton of concentrate to improve the selectivity of the flotation operation.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A method for flotation of scale graphite ore comprises the following steps:
(1) carrying out high-pressure roller milling on the flake graphite raw ore to obtain crushed raw ore; mixing the crushed raw ore with a collecting agent, a foaming agent, a pH control agent and an inhibitor, and performing roughing operation to obtain roughed tailings and roughed concentrate;
(2) stirring and grinding the rough concentration obtained in the step (1), and then carrying out concentration operation to obtain concentrated tailings and concentrated concentrate;
(3) repeating the operation of the concentration operation after the stirring and grinding in the step (2) on the concentration concentrate obtained in the step (2) to obtain final concentrate and final tailings; the repetition frequency is 1-3 times;
and (3) the flotation column used in the concentration operation in the step (2) and the step (3) is a static micro-bubble cyclone flotation column.
2. The flotation method for flake graphite ore according to claim 1, wherein the mass percentage of the crushed raw ore in the step (1) with the grain diameter of-0.074 mm is 60-70%.
3. The method for floating crystalline flake graphite ore according to claim 1, wherein the amount of the collecting agent, the amount of the foaming agent and the amount of the inhibitor in the step (1) are respectively 300-400 g/t, 300-400 g/t and 1200-1500 g/t, respectively, based on the mass of the crushed raw ore; the pH value of the ore pulp in the roughing operation process is controlled to be 10-11, and the mass concentration of the ore pulp is 5-10%.
4. The flotation method for flake graphite ore according to claim 1, wherein the mass percentage of the product obtained by stirring and grinding in step (2) and having the grain diameter of-0.074 mm is 80-85%.
5. The flotation method for flake graphite ore according to claim 1, wherein the product obtained by stirring and grinding in the step (3) has a mass percentage content of 74-78% with a grain size of-0.074 mm.
6. The flotation method for flake graphite ore according to claim 1, wherein the particle size of the grinding medium used in the stirring mill in the step (2) and the step (3) is 2-5 mm.
7. The flotation method for flake graphite ore according to claim 3, wherein during the concentration operation of step (2), the pH value of ore pulp is controlled to be 10-11; adding foaming agent in the fine selection process; the addition amount of the foaming agent is 500-600 g/t on the basis of the mass of the crushed raw ore.
8. The flotation method for flake graphite ore according to claim 3, wherein during the concentration operation of step (3), the pH value of ore pulp is controlled to be 10-11; adding foaming agent in the fine selection process; the addition amount of the foaming agent is 800-1000 g/t on the basis of the mass of the crushed raw ore.
9. The method for flotation of crystalline flake graphite ore according to claim 1, wherein the feeding speed of the flotation column in the roughing operation in step (1) and the concentrating operation in step (2) is 0.6-0.8L/min, and the feeding speed of the flotation column in the concentrating operation in step (3) is 0.4-0.5L/min.
10. The method for floating crystalline flake graphite ore according to claim 1, wherein the aeration amount in the roughing operation in the step (1), the concentration operation in the step (2) and the concentration operation in the step (3) is independently 0.8 to 1.2L/min, the thickness of the foam layer is independently 25 to 30cm, and the flow rate of the washing water is independently 0.3 to 0.5L/min.
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