CN113083493A - Microwave roasting pretreatment graphite ore enhanced flotation purification method - Google Patents
Microwave roasting pretreatment graphite ore enhanced flotation purification method Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 167
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 145
- 239000010439 graphite Substances 0.000 title claims abstract description 145
- 238000005188 flotation Methods 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000000746 purification Methods 0.000 title claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 21
- 239000012141 concentrate Substances 0.000 claims description 112
- 239000003795 chemical substances by application Substances 0.000 claims description 84
- 239000004088 foaming agent Substances 0.000 claims description 72
- 239000002245 particle Substances 0.000 claims description 64
- 239000003350 kerosene Substances 0.000 claims description 50
- 238000000227 grinding Methods 0.000 claims description 42
- 230000002000 scavenging effect Effects 0.000 claims description 18
- 239000004115 Sodium Silicate Substances 0.000 claims description 14
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 14
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000001238 wet grinding Methods 0.000 claims description 8
- 238000004513 sizing Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 6
- 239000011707 mineral Substances 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 238000010494 dissociation reaction Methods 0.000 description 4
- 230000005593 dissociations Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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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
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B7/00—Combinations of wet processes or apparatus with other processes or apparatus, e.g. for dressing ores or garbage
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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
- B03D1/002—Inorganic 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
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/008—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
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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
- 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
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/04—Frothers
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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 relates to a microwave roasting pretreatment graphite ore enhanced flotation purification method, and belongs to the technical field of graphite purification. The invention aims at the difficult-to-float low-grade fine flake graphite ore to carry out microwave roasting pretreatment and enhanced flotation so as to improve the graphite purification effect, the fixed carbon content of the graphite ore is 5-20%, the main impurities are oxides of elements such as Fe, Al, Ca, Mg, Si and the like, the water content is below 1%, the graphite ore is pretreated for 5-30 min by microwave roasting, and then the graphite ore is crushed, wet-ground and floated for multiple times so as to obtain a graphite product with the fixed carbon content of 95-97%. The method can effectively purify the graphite ore, so that the graphite meets the production requirement, and the purification method has the advantages of low energy consumption, simple operation, high product purity, easy realization of industrialization and the like.
Description
Technical Field
The invention relates to a microwave roasting pretreatment graphite ore enhanced flotation purification method, and belongs to the technical field of graphite purification.
Background
The graphite has excellent physical and chemical properties such as high temperature resistance, heat and electricity conduction, stable chemical property, good lubricity and the like, and is an important and widely-used non-metallic mineral material and raw material. With the continuous expansion of the application field of graphite in recent years, various novel graphite materials, such as graphene materials, lithium ion battery negative electrode materials, spherical graphite, nano graphite and the like, are researched by taking graphite as a raw material. However, at present, because the graphite has wide application and the use amount is increased year by year, and the graphite ore resources, particularly the easily selected high-quality flake graphite resources are continuously reduced, the reasonable development of the low-grade fine flake graphite resources with larger reserves and poorer quality in China becomes a necessary trend. However, because the low-grade fine flake graphite mineral has complex composition and fine embedding characteristics, and belongs to low-quality refractory graphite, the low-grade fine flake graphite mineral can be purified by the existing flotation technology, but the purity is usually only 85-95%.
In the prior art, the method for improving the flotation efficiency of the fine-particle graphite promotes the dissociation of the fine-particle microcrystalline graphite by using a multi-stage vertical mill process, so that the flotation efficiency of the fine-particle graphite is improved, although the medicament amount is reduced and the selection times are reduced, the final fixed carbon content of the graphite ore is only 85-93%, and the requirement of actual production cannot be met. The combined collector for flotation of cryptocrystalline graphite ore improves the flotation effect of graphite ore through the combined collector, and although higher-grade graphite ore is obtained, the preparation of the composite collector can be changed due to slight change of mineral properties, so that the combined collector is not suitable for large-scale popularization and application. The fine flake-cryptocrystalline mixed graphite beneficiation process adopts gradually reduced low concentration in multiple concentration processes, and ensures mineral dispersibility, so that the flotation effect is improved, but the method is complicated to operate, the final grade is only about 91%, and the production requirement cannot be completely met.
At present, the technology of good purification effect of low-grade fine flake graphite has high cost and relatively complex process; the low-cost purification technology has low purification effect, and cannot obtain graphite with high fixed carbon content.
Disclosure of Invention
The invention provides a method for strengthening, floating and purifying graphite ore by microwave roasting pretreatment, aiming at the problems that the low-grade fine-scale graphite ore has very fine embedded particle size, the crystal particle size is far lower than the lower limit of mineral flotation particle size, the flotation effect is poor, the embedded particle size is not uniform, and the monomer dissociation is difficult in the prior art.
A microwave roasting pretreatment graphite ore enhanced flotation purification method comprises the following specific steps:
(1) crushing low-grade fine flake graphite ore to the particle size of 0.83-1.7 mm to obtain graphite ore particles A, and carrying out microwave roasting pretreatment on the graphite ore particles A for 5-30 min to obtain graphite ore particles B;
(2) carrying out wet grinding treatment on the graphite ore particles B in the step (1) until the particle size of the graphite ore particles B is not more than 0.075mm and accounts for 80-90% of the particle size of the graphite ore particles B to obtain flotation graphite ore pulp;
(3) adding a foaming agent A1, a collecting agent A2 and an adjusting agent A3 into the flotation graphite ore pulp for roughing, and adding a foaming agent A1, a collecting agent A2 and an adjusting agent A3 for scavenging to obtain a middling ore I, a rough concentrate and a tailing I; adding a foaming agent A1 and a collecting agent A2 into the rough concentrate for primary concentration to obtain a middling II and a concentrate I; after the concentrate is ground, adding a foaming agent A1 and a collecting agent A2 for secondary concentration to obtain a middling III and a concentrate II; after the second concentrate is ground, adding a foaming agent A1 and a collecting agent A2 for three times of concentration to obtain a fourth middling and a third concentrate; after the third concentrate is subjected to grinding treatment, adding a foaming agent A1 and a collecting agent A2 for four-time concentration to obtain a fifth middling and a fourth concentrate; after grinding the concentrate IV, adding a foaming agent A1 and a collecting agent A2 to carry out five-time concentration to obtain a middling six and a concentrate five; grinding the concentrate five, and then adding a foaming agent A1 and a collecting agent A2 to carry out six-time concentration to obtain a middling seven and a concentrate six; combining the first middling ore, the second middling ore and the third middling ore, returning to perform roughing and scavenging, combining the fourth middling ore, the fifth middling ore, the sixth middling ore and the seventh middling ore, returning to perform primary concentration to form a closed loop, and repeating closed flotation for 3-5 times;
(4) filtering and drying the concentrate six in the step (3) to obtain a graphite product;
the fixed carbon content of the graphite ore in the step (1) is 1-10%;
the foaming agent A1 in the step (3) is No. two oil, the collecting agent A2 is kerosene, and the regulator A3 is sodium silicate;
further, the adding amount of a foaming agent A1 in the rough concentration is 50-100 g/t, the adding amount of a collecting agent A2 is 200-400 g/t, and the adding amount of a regulator A3 is 1000-1500 g/t; the adding amount of the foaming agent A1 in the scavenging process is 25-50 g/t, the adding amount of the collecting agent A2 is 100-200 g/t, and the adding amount of the regulator A3 is 500-800 g/t; the adding amount of the foaming agent A1 in the fine selection is 10-30 g/t, and the adding amount of the collecting agent A2 is 50-100 g/t;
the ore grinding treatment time in the step (3) is 5-10 min, and the ore pulp concentration during the ore grinding treatment is 35-45%;
the fixed carbon content of the low-grade fine flake graphite is 5-20%, the main components of impurities are oxides of elements such as Fe, Al, Ca, Mg, Si and the like, and the water content is below 1%;
the fixed carbon content of the graphite product is 95-97%.
The invention has the beneficial effects that:
(1) according to the invention, the low-grade fine flake graphite ore is pretreated by microwave roasting, so that the dissociation of the low-grade fine flake graphite ore during subsequent ore grinding is promoted, the dissociation degree is improved, the flotation effect is improved, the ore grinding time is reduced, the energy consumption is reduced, and the machine abrasion is reduced;
(2) in the selection process, the multi-section ore grinding treatment is performed, so that the graphite ore is fully dissociated in the multi-section ore grinding, and the flotation effect is improved;
(3) the graphite product has high grade, the fixed carbon content can reach 95-97%, and the requirement of subsequent graphite processing and production can be met.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: a microwave roasting pretreatment graphite ore enhanced flotation purification method (see figure 1) comprises the following specific steps:
(1) crushing the low-grade fine flake graphite ore to the particle size of 0.83-1.7 mm to obtain graphite ore particles A, and carrying out microwave roasting pretreatment on the graphite ore particles A for 5min to obtain graphite ore particles B; wherein the fixed carbon content of the low-grade fine flake graphite ore is 5.63 percent, the main components of impurities are oxides of elements such as Fe, Al, Ca, Mg, Si and the like, and the water content is below 1 percent;
(2) carrying out wet grinding treatment on the graphite ore particles B in the step (1) until the particle size of the graphite ore particles B is not more than 0.075mm and accounts for 86% to obtain flotation graphite ore pulp;
(3) adding 90g/t of foaming agent A1 (second oil), 360g/t of collecting agent A2 (kerosene) and 1000g/t of adjusting agent A3 (sodium silicate) into the flotation graphite ore pulp for roughing, adding 45g/t of foaming agent A1 (second oil), 180g/t of collecting agent A2 (kerosene) and 500g/t of adjusting agent A3 (sodium silicate) for scavenging, and obtaining middling ore I, rough concentrate and tailing I; adding 20g/t of foaming agent A1 (second oil) and 90g/t of collecting agent A2 (kerosene) into the rough concentrate for primary concentration to obtain middling II and concentrate I; after the concentrate is ground for 6min, 20g/t of foaming agent A1 (No. two oil) and 90g/t of collecting agent A2 (kerosene) are added for secondary concentration to obtain middling III and concentrate II; after the second concentrate is ground for 6min, 20g/t of foaming agent A1 (second oil) and 90g/t of collecting agent A2 (kerosene) are added for three times of concentration, and a fourth middling and a third concentrate are obtained; grinding the concentrate III for 6min, and then adding 20g/t of foaming agent A1 (No. two oil) and 90g/t of collecting agent A2 (kerosene) to carry out four-time concentration to obtain middling five and concentrate IV; grinding the concentrate IV for 6min, and adding 20g/t foaming agent A1 (No. two oil) and 90g/t collecting agent A2 (kerosene) for five-time concentration to obtain six middlings and five concentrate; grinding the concentrate five for 6min, and then adding 20g/t foaming agent A1 (No. two oil) and 90g/t collecting agent A2 (kerosene) for six times of concentration to obtain Chinese middling seven and concentrate six; combining the first middling ore, the second middling ore and the third middling ore, returning to perform roughing and scavenging, combining the fourth middling ore, the fifth middling ore, the sixth middling ore and the seventh middling ore, returning to perform primary concentration to form a closed loop, and repeating closed flotation for 3-5 times; wherein the concentration of the ore pulp is 40% of the concentration of ore grinding during the ore grinding treatment;
(4) filtering and drying the concentrate six in the step (3) to obtain a graphite product;
the graphite product of this example had a fixed carbon content of 96.17% and a recovery of 94.25%.
Example 2: a microwave roasting pretreatment graphite ore enhanced flotation purification method (see figure 1) comprises the following specific steps:
(1) crushing low-grade fine flake graphite ore to the particle size of 0.83-1.7 mm to obtain graphite ore particles A, and carrying out microwave roasting pretreatment on the graphite ore particles A for 10min to obtain graphite ore particles B; wherein the fixed carbon content of the low-grade fine flake graphite ore is 5.63 percent, the main components of impurities are oxides of elements such as Fe, Al, Ca, Mg, Si and the like, and the water content is below 1 percent;
(2) carrying out wet grinding treatment on the graphite ore particles B in the step (1) until the particle size of the graphite ore particles B is not more than 0.075mm and accounts for 84% to obtain flotation graphite ore pulp;
(3) adding 60g/t of foaming agent A1 (second oil), 300g/t of collecting agent A2 (kerosene) and 1200g/t of adjusting agent A3 (sodium silicate) into the flotation graphite ore pulp for roughing, adding 30g/t of foaming agent A1 (second oil), 150g/t of collecting agent A2 (kerosene) and 600g/t of adjusting agent A3 (sodium silicate) for scavenging, and obtaining middling ore I, rough concentrate and tailing I; adding 15g/t of foaming agent A1 (second oil) and 80g/t of collecting agent A2 (kerosene) into the rough concentrate for primary concentration to obtain middling II and concentrate I; after the concentrate is ground for 6min, 15g/t of foaming agent A1 (No. two oil) and 80g/t of collecting agent A2 (kerosene) are added for secondary concentration to obtain middling III and concentrate II; after the second concentrate is ground for 6min, 15g/t of foaming agent A1 (second oil) and 80g/t of collecting agent A2 (kerosene) are added for three times of concentration, and a fourth middling and a third concentrate are obtained; grinding the concentrate III for 6min, and then adding 15g/t of foaming agent A1 (second oil) and 80g/t of collecting agent A2 (kerosene) for four-time concentration to obtain middling five and concentrate IV; grinding the concentrate IV for 6min, and adding 15g/t foaming agent A1 (No. two oil) and 80g/t collecting agent A2 (kerosene) for five-time concentration to obtain six middlings and five concentrates; grinding the concentrate five for 7min, and then adding 15g/t foaming agent A1 (No. two oil) and 80g/t collecting agent A2 (kerosene) for six times of concentration to obtain Chinese middling seven and concentrate six; combining the first middling ore, the second middling ore and the third middling ore, returning to perform roughing and scavenging, combining the fourth middling ore, the fifth middling ore, the sixth middling ore and the seventh middling ore, returning to perform primary concentration to form a closed loop, and repeating closed flotation for 3-5 times; wherein the concentration of the ore pulp is 35% of the concentration of ore grinding during the ore grinding treatment;
(4) filtering and drying the concentrate six in the step (3) to obtain a graphite product;
the graphite product of this example had a fixed carbon content of 96.28% and a recovery of 94.57%.
Example 3: a microwave roasting pretreatment graphite ore enhanced flotation purification method (see figure 1) comprises the following specific steps:
(1) crushing low-grade fine flake graphite ore to the particle size of 0.83-1.7 mm to obtain graphite ore particles A, and carrying out microwave roasting pretreatment on the graphite ore particles A for 20min to obtain graphite ore particles B; wherein the fixed carbon content of the low-grade fine flake graphite ore is 5.63 percent, the main components of impurities are oxides of elements such as Fe, Al, Ca, Mg, Si and the like, and the water content is below 1 percent;
(2) carrying out wet grinding treatment on the graphite ore particles B in the step (1) until the particle size of the graphite ore particles B is not more than 0.075mm and accounts for 84% to obtain flotation graphite ore pulp;
(3) adding 80g/t of foaming agent A1 (second oil), 250g/t of collecting agent A2 (kerosene) and 1100g/t of regulator A3 (sodium silicate) into the flotation graphite ore pulp for roughing, adding 40g/t of foaming agent A1 (second oil), 125g/t of collecting agent A2 (kerosene) and 550g/t of regulator A3 (sodium silicate) for scavenging, and obtaining middling ore I, rough concentrate and tailing I; adding 18g/t of foaming agent A1 (second oil) and 90g/t of collecting agent A2 (kerosene) into the rough concentrate for primary concentration to obtain middling II and concentrate I; after the concentrate is ground for 5min, adding 18g/t of foaming agent A1 (No. two oil) and 90g/t of collecting agent A2 (kerosene) for secondary concentration to obtain middling III and concentrate II; after the second concentrate is ground for 5min, adding 18g/t of foaming agent A1 (second oil) and 90g/t of collecting agent A2 (kerosene) for three-time concentration to obtain a fourth middling and a third concentrate; after the concentrate III is ground for 5min, adding 18g/t of foaming agent A1 (No. two oil) and 90g/t of collecting agent A2 (kerosene) for four-time concentration to obtain middling five and concentrate IV; grinding the concentrate four for 5min, and adding 18g/t foaming agent A1 (No. two oil) and 90g/t collecting agent A2 (kerosene) for five-time concentration to obtain six middlings and five concentrate; grinding the concentrate five for 5min, and then adding 18g/t foaming agent A1 (No. two oil) and 90g/t collecting agent A2 (kerosene) for six times of concentration to obtain Chinese middling seven and concentrate six; combining the first middling ore, the second middling ore and the third middling ore, returning to perform roughing and scavenging, combining the fourth middling ore, the fifth middling ore, the sixth middling ore and the seventh middling ore, returning to perform primary concentration to form a closed loop, and repeating closed flotation for 3-5 times; wherein the concentration of the ore pulp is 38 percent of the concentration of ore grinding during the ore grinding treatment;
(4) filtering and drying the concentrate six in the step (3) to obtain a graphite product;
the graphite product of this example had a fixed carbon content of 96.38% and a recovery of 94.63%.
Example 4: a microwave roasting pretreatment graphite ore enhanced flotation purification method (see figure 1) comprises the following specific steps:
(1) crushing the low-grade fine flake graphite ore to the particle size of 0.83-1.7 mm to obtain graphite ore particles A, and carrying out microwave roasting pretreatment on the graphite ore particles A for 25min to obtain graphite ore particles B; wherein the fixed carbon content of the low-grade fine flake graphite ore is 5.63 percent, the main components of impurities are oxides of elements such as Fe, Al, Ca, Mg, Si and the like, and the water content is below 1 percent;
(2) carrying out wet grinding treatment on the graphite ore particles B in the step (1) until the particle size of the graphite ore particles B is not more than 0.075mm and accounts for 86% to obtain flotation graphite ore pulp;
(3) adding 90g/t of foaming agent A1 (second oil), 360g/t of collecting agent A2 (kerosene) and 1000g/t of adjusting agent A3 (sodium silicate) into the flotation graphite ore pulp for roughing, adding 45g/t of foaming agent A1 (second oil), 180g/t of collecting agent A2 (kerosene) and 500g/t of adjusting agent A3 (sodium silicate) for scavenging, and obtaining middling ore I, rough concentrate and tailing I; adding 20g/t of foaming agent A1 (second oil) and 90g/t of collecting agent A2 (kerosene) into the rough concentrate for primary concentration to obtain middling II and concentrate I; after the concentrate is ground for 6min, 20g/t of foaming agent A1 (No. two oil) and 90g/t of collecting agent A2 (kerosene) are added for secondary concentration to obtain middling III and concentrate II; after the second concentrate is ground for 6min, 20g/t of foaming agent A1 (second oil) and 90g/t of collecting agent A2 (kerosene) are added for three times of concentration, and a fourth middling and a third concentrate are obtained; grinding the concentrate III for 6min, and then adding 20g/t of foaming agent A1 (No. two oil) and 90g/t of collecting agent A2 (kerosene) to carry out four-time concentration to obtain middling five and concentrate IV; grinding the concentrate IV for 6min, and adding 20g/t foaming agent A1 (No. two oil) and 90g/t collecting agent A2 (kerosene) for five-time concentration to obtain six middlings and five concentrate; grinding the concentrate five for 6min, and then adding 20g/t foaming agent A1 (No. two oil) and 90g/t collecting agent A2 (kerosene) for six times of concentration to obtain Chinese middling seven and concentrate six; combining the first middling ore, the second middling ore and the third middling ore, returning to perform roughing and scavenging, combining the fourth middling ore, the fifth middling ore, the sixth middling ore and the seventh middling ore, returning to perform primary concentration to form a closed loop, and repeating closed flotation for 3-5 times; wherein the concentration of the ore pulp is 40% of the concentration of ore grinding during the ore grinding treatment;
(4) filtering and drying the concentrate six in the step (3) to obtain a graphite product;
the graphite product of this example had a fixed carbon content of 96.41% and a recovery of 94.62%.
Example 5: a microwave roasting pretreatment graphite ore enhanced flotation purification method (see figure 1) comprises the following specific steps:
(1) crushing low-grade fine flake graphite ore to the particle size of 0.83-1.7 mm to obtain graphite ore particles A, and carrying out microwave roasting pretreatment on the graphite ore particles A for 30min to obtain graphite ore particles B; wherein the fixed carbon content of the low-grade fine flake graphite ore is 5.63 percent, the main components of impurities are oxides of elements such as Fe, Al, Ca, Mg, Si and the like, and the water content is below 1 percent;
(2) carrying out wet grinding treatment on the graphite ore particles B in the step (1) until the particle size of the graphite ore particles B is not more than 0.075mm and accounts for 86% to obtain flotation graphite ore pulp;
(3) adding 70g/t of foaming agent A1 (second oil), 320g/t of collecting agent A2 (kerosene) and 1400g/t of adjusting agent A3 (sodium silicate) into the flotation graphite ore pulp for roughing, adding 35g/t of foaming agent A1 (second oil), 160g/t of collecting agent A2 (kerosene) and 700g/t of adjusting agent A3 (sodium silicate) for scavenging, and obtaining middling ore I, rough concentrate and tailing I; adding 25g/t of foaming agent A1 (second oil) and 85g/t of collecting agent A2 (kerosene) into the rough concentrate for primary concentration to obtain middling II and concentrate I; after the concentrate is ground for 6min, adding 25g/t of foaming agent A1 (No. two oil) and 85g/t of collecting agent A2 (kerosene) for secondary concentration to obtain middling III and concentrate II; after the second concentrate is ground for 6min, 25g/t of foaming agent A1 (second oil) and 85g/t of collecting agent A2 (kerosene) are added for three times of concentration, and a fourth middling and a third concentrate are obtained; after the concentrate III is ground for 6min, 25g/t of foaming agent A1 (second oil) and 85g/t of collecting agent A2 (kerosene) are added for four-time concentration, and middling five and concentrate IV are obtained; grinding the concentrate IV for 6min, and adding 25g/t foaming agent A1 (No. two oil) and 85g/t collecting agent A2 (kerosene) for five-time concentration to obtain six middlings and five concentrate; grinding the concentrate five for 6min, and then adding 25g/t foaming agent A1 (No. two oil) and 85g/t collecting agent A2 (kerosene) for six times of concentration to obtain Chinese middling seven and concentrate six; combining the first middling ore, the second middling ore and the third middling ore, returning to perform roughing and scavenging, combining the fourth middling ore, the fifth middling ore, the sixth middling ore and the seventh middling ore, returning to perform primary concentration to form a closed loop, and repeating closed flotation for 3-5 times; wherein the concentration of the ore pulp is 40% of the concentration of ore grinding during the ore grinding treatment;
(4) filtering and drying the concentrate six in the step (3) to obtain a graphite product;
the graphite product of this example had a fixed carbon content of 95.38% and a recovery of 93.63%.
Example 6: a microwave roasting pretreatment graphite ore enhanced flotation purification method (see figure 1) comprises the following specific steps:
(1) crushing low-grade fine flake graphite ore to the particle size of 0.83-1.7 mm to obtain graphite ore particles A, and carrying out microwave roasting pretreatment on the graphite ore particles A for 20min to obtain graphite ore particles B; wherein the fixed carbon content of the low-grade fine flake graphite ore is 5.63 percent, the main components of impurities are oxides of elements such as Fe, Al, Ca, Mg, Si and the like, and the water content is below 1 percent;
(2) carrying out wet grinding treatment on the graphite ore particles B in the step (1) until the particle size of the graphite ore particles B is not more than 0.075mm and accounts for 85% to obtain flotation graphite ore pulp;
(3) adding 90g/t of foaming agent A1 (second oil), 200g/t of collecting agent A2 (kerosene) and 1000g/t of regulator A3 (sodium silicate) into the flotation graphite ore pulp for roughing, adding 45g/t of foaming agent A1 (second oil), 100g/t of collecting agent A2 (kerosene) and 500g/t of regulator A3 (sodium silicate) for scavenging, and obtaining middling ore I, rough concentrate and tailing I; adding 20g/t of foaming agent A1 (second oil) and 50g/t of collecting agent A2 (kerosene) into the rough concentrate for primary concentration to obtain middling II and concentrate I; after the concentrate is ground for 6min, 20g/t of foaming agent A1 (No. two oil) and 50g/t of collecting agent A2 (kerosene) are added for secondary concentration to obtain middling III and concentrate II; after the second concentrate is ground for 6min, 20g/t of foaming agent A1 (second oil) and 50g/t of collecting agent A2 (kerosene) are added for three times of concentration, and a fourth middling and a third concentrate are obtained; grinding the concentrate III for 6min, and then adding 20g/t of foaming agent A1 (No. two oil) and 50g/t of collecting agent A2 (kerosene) to carry out four-time concentration to obtain middling five and concentrate IV; grinding the concentrate IV for 6min, and adding 20g/t foaming agent A1 (No. two oil) and 50g/t collecting agent A2 (kerosene) for five-time concentration to obtain six middlings and five concentrates; grinding the concentrate five for 6min, and then adding 20g/t foaming agent A1 (No. two oil) and 50g/t collecting agent A2 (kerosene) for six times of concentration to obtain Chinese middling seven and concentrate six; combining the first middling ore, the second middling ore and the third middling ore, returning to perform roughing and scavenging, combining the fourth middling ore, the fifth middling ore, the sixth middling ore and the seventh middling ore, returning to perform primary concentration to form a closed loop, and repeating closed flotation for 3-5 times; wherein the concentration of the ore pulp is 40% of the concentration of ore grinding during the ore grinding treatment;
(4) filtering and drying the concentrate six in the step (3) to obtain a graphite product;
the graphite product of this example had a fixed carbon content of 95.46% and a recovery of 94.13%.
While the present invention has been described in detail with reference to the specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
Claims (5)
1. A microwave roasting pretreatment graphite ore enhanced flotation purification method is characterized by comprising the following specific steps:
(1) crushing low-grade fine flake graphite ore to the particle size of 0.83-1.7 mm to obtain graphite ore particles A, and carrying out microwave roasting pretreatment on the graphite ore particles A for 5-30 min to obtain graphite ore particles B;
(2) carrying out wet grinding treatment on the graphite ore particles B in the step (1) until the particle size of the graphite ore particles B is not more than 0.075mm and accounts for 80-90% of the particle size of the graphite ore particles B to obtain flotation graphite ore pulp;
(3) adding a foaming agent A1, a collecting agent A2 and an adjusting agent A3 into the flotation graphite ore pulp for roughing, and adding a foaming agent A1, a collecting agent A2 and an adjusting agent A3 for scavenging to obtain a middling ore I, a rough concentrate and a tailing I; adding a foaming agent A1 and a collecting agent A2 into the rough concentrate for primary concentration to obtain a middling II and a concentrate I; after the concentrate is ground, adding a foaming agent A1 and a collecting agent A2 for secondary concentration to obtain a middling III and a concentrate II; after the second concentrate is ground, adding a foaming agent A1 and a collecting agent A2 for three times of concentration to obtain a fourth middling and a third concentrate; after the third concentrate is subjected to grinding treatment, adding a foaming agent A1 and a collecting agent A2 for four-time concentration to obtain a fifth middling and a fourth concentrate; after grinding the concentrate IV, adding a foaming agent A1 and a collecting agent A2 to carry out five-time concentration to obtain a middling six and a concentrate five; grinding the concentrate five, and then adding a foaming agent A1 and a collecting agent A2 to carry out six-time concentration to obtain a middling seven and a concentrate six; combining the first middling ore, the second middling ore and the third middling ore, returning to perform roughing and scavenging, combining the fourth middling ore, the fifth middling ore, the sixth middling ore and the seventh middling ore, returning to perform primary concentration to form a closed loop, and repeating closed flotation for 3-5 times;
(4) and (4) filtering and drying the concentrate six in the step (3) to obtain a graphite product.
2. The microwave roasting pretreatment graphite ore enhanced flotation purification method according to claim 1, characterized in that: the fixed carbon content of the graphite ore in the step (1) is 1-10%.
3. The microwave roasting pretreatment graphite ore enhanced flotation purification method according to claim 1, characterized in that: in the step (3), the foaming agent A1 is No. two oil, the collecting agent A2 is kerosene, and the regulator A3 is sodium silicate.
4. The microwave roasting pretreatment graphite ore enhanced flotation purification method according to claim 3, characterized in that: the adding amount of the foaming agent A1 in the rough sizing is 50-100 g/t, the adding amount of the collecting agent A2 is 200-400 g/t, and the adding amount of the regulator A3 is 1000-1500 g/t; the adding amount of the foaming agent A1 in the scavenging process is 25-50 g/t, the adding amount of the collecting agent A2 is 100-200 g/t, and the adding amount of the regulator A3 is 500-800 g/t; the adding amount of the foaming agent A1 in the fine selection is 10-30 g/t, and the adding amount of the collecting agent A2 is 50-100 g/t.
5. The microwave roasting pretreatment graphite ore enhanced flotation purification method according to claim 1, characterized in that: and (3) grinding for 5-10 min, wherein the concentration of the ore pulp during grinding is 35-45%.
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