CN111054520A - Method for improving recovery rate of titanium concentrate through pulse microwave pretreatment - Google Patents

Method for improving recovery rate of titanium concentrate through pulse microwave pretreatment Download PDF

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Publication number
CN111054520A
CN111054520A CN201911094663.3A CN201911094663A CN111054520A CN 111054520 A CN111054520 A CN 111054520A CN 201911094663 A CN201911094663 A CN 201911094663A CN 111054520 A CN111054520 A CN 111054520A
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microwave pretreatment
titanium
titanium concentrate
recovery rate
concentrate
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CN201911094663.3A
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Chinese (zh)
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郭胜惠
侯明
杨黎
高冀芸
胡途
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03CMAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C1/00Magnetic separation
    • B03C1/02Magnetic separation acting directly on the substance being separated
    • B03C1/30Combinations with other devices, not otherwise provided for
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03CMAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C1/00Magnetic separation
    • B03C1/005Pretreatment specially adapted for magnetic separation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03CMAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C1/00Magnetic separation
    • B03C1/02Magnetic separation acting directly on the substance being separated
    • B03C1/025High gradient magnetic separators
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation

Abstract

The invention discloses a method for improving the recovery rate of titanium concentrate by pulse microwave pretreatment, which comprises the steps of pulse microwave pretreatment, ore grinding, magnetic separation and flotation, wherein low-grade coated ilmenite is placed in a pulse microwave oven for pulse microwave pretreatment, the pretreated ore is placed in a ball mill for ore grinding after being cooled to room temperature, the treated ore is subjected to strong magnetic iron removal to obtain strong magnetic concentrate, and the obtained strong magnetic concentrate is subjected to flotation to obtain the titanium concentrate. The invention utilizes the difference of dielectric constants of gangue and concentrate to generate stress difference at different phase interfaces in the mineral, thereby achieving the effect of cracking the mineral before grinding, after the process, the content of iron in the titanium concentrate is the lowest, the precision of the titanium concentrate is greatly increased, the recovery rate of the titanium concentrate is improved, the low-intensity magnetic separation process and the gravity separation process are omitted, meanwhile, the pulse microwave only has microsecond width, and the average power is only kilowatt level, thus the invention is a new high-efficiency, low-consumption and energy-saving beneficiation method.

Description

Method for improving recovery rate of titanium concentrate through pulse microwave pretreatment
Technical Field
The invention relates to the field of mineral separation flotation, in particular to a method for improving the recovery rate of titanium concentrate through pulse microwave pretreatment.
Background
Titanium and its alloys have excellent physicochemical properties, which have been widely noticed and developed by people. Titanium resources mainly depend on development and acquisition of ilmenite, and it is worth mentioning that the ilmenite resource reserve in China is the first in the world, and the primary ilmenite is taken as the main resource, and accounts for 94.5% of the resource. However, although the total amount of the titanium resource is large, the titanium resource has a fine embedded particle size and a high content of calcium and magnesium in crystal lattices, and belongs to a wrapping type mineral. Ilmenite has been greatly limited in its exploitation applications.
At present, the method for treating ilmenite and recovering titanium concentrate at home is 'strong magnetism-gravity separation-ore grinding classification-weak magnetism-flotation'. The process is limited to the case of high grade (> 8.5%) of TiO2 in the raw ore. For minerals with low taste, the method is difficult to realize high titanium concentrate recovery rate, and meanwhile, because the raw ore has fine granularity and is wrapped by other impurities, high-grade titanium concentrate is difficult to obtain. Therefore, the development of a method for enriching ilmenite, which can ensure high recovery rate of titanium and high grade of TiO2, has great significance.
Disclosure of Invention
The invention aims to provide a method for improving the recovery rate of titanium concentrate by pulse microwave pretreatment, so as to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following scheme: the invention provides a method for improving the recovery rate of titanium concentrate by pulse microwave pretreatment, which comprises the following steps:
(1) pulse microwave pretreatment: paving the low-grade coated ilmenite in pulse microwave equipment for pulse microwave pretreatment;
(2) grinding: placing the pretreated minerals in a ball mill;
(3) magnetic separation: carrying out strong magnetic iron removal on the ground minerals to obtain strong magnetic titanium concentrate;
(4) flotation: and carrying out flotation on the strong magnetic concentrate to obtain the titanium concentrate.
Preferably, in the pulse microwave pretreatment, the pulse frequency is 400-700Hz, the instantaneous power applied to the low-grade coated ilmenite is 40-90MW, the pulse width is 4-10 mus, and the irradiation time is 10-20 s.
Preferably, in the ore grinding, the rotating speed of the ball mill is 300-700r/min, and the ball milling is carried out for 4-8 h.
Preferably, in the magnetic separation, the magnetic field intensity of the strong magnetic iron removal is 0.5-1.2T.
Preferably, the flotation comprises sulfur floating and titanium floating, the sulfur floating adopts a primary coarse sweeping flow and a secondary sweeping flow, and the titanium floating adopts a primary coarse sweeping flow, a secondary sweeping flow and a secondary fine sweeping flow.
Preferably, the dosage of the sulfuric acid in the sulfur floating process is 500g/t, and the dosage of the No. 2 oil is 60 g/t.
Preferably, the using amount of the collecting agent in the floating titanium is 1800g/h, and the using amount of the regulator is 1200 g/t; in the two refining processes, the addition amount of the first sulfuric acid is 350g/t, and the addition amount of the second sulfuric acid is 200 g/t.
The invention discloses the following technical effects: the invention utilizes the difference of dielectric constants of gangue and concentrate to generate stress difference at different phase interfaces in the mineral, thereby achieving the effect of cracking the mineral before grinding, and after grinding, magnetic separation and flotation, the content of iron in the titanium concentrate is the lowest, thereby greatly increasing the precision of the titanium concentrate and improving the recovery rate of the titanium concentrate.
Drawings
FIG. 1 is a relation between the instantaneous power of pulse microwave and the yield of ilmenite;
FIG. 2 is a relationship between the instantaneous power of the pulsed microwave and the taste of ilmenite;
FIG. 3 is the relationship between the irradiation time of the pulse microwave and the yield of ilmenite;
FIG. 4 is the relationship between the irradiation time of the pulsed microwave and the taste of ilmenite.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
The invention provides a method for improving the recovery rate of titanium concentrate by pulse microwave pretreatment, which comprises the following steps:
(1) pulse microwave pretreatment: flatly paving the low-grade coated ilmenite in pulse microwave equipment, performing pulse microwave pretreatment, cooling to room temperature, and then placing the pretreated mineral in a ball mill for ore grinding treatment;
(2) grinding: placing the pretreated minerals in a ball mill;
(3) magnetic separation: carrying out strong magnetic iron removal on the ground minerals to obtain strong magnetic titanium concentrate;
(4) flotation: and carrying out flotation on the strong magnetic concentrate to obtain the titanium concentrate.
Referring to fig. 1-4, the invention obtains the relationship between each parameter and the yield and the taste through experiments, the taste and the yield of the obtained titanium concentrate are in direct proportion to the set parameters (pulse microwave frequency, instantaneous power, pulse width, irradiation time, ball mill rotating speed and ball milling time) of the pulse microwave pretreated ore, when the taste and the yield are closer to 100%, the change of the parameters of the pulse microwave pretreated ore has little influence on the taste and the yield, the problems of energy conservation and the like are considered, and the set parameters of the pulse microwave pretreated ore are appropriate.
In the further optimization scheme, in the pulse microwave pretreatment, the pulse frequency is 400-700Hz, the instantaneous power added on the low-grade coated ilmenite is 40-90MW, the pulse width is 4-10 mus, and the irradiation time is 10-20 s.
Further optimizing the scheme, in the ore grinding, the rotating speed of the ball mill is 300-.
In the further optimized scheme, the magnetic field intensity of the strong magnetic deironing is 0.5-1.2T in the magnetic separation.
According to a further optimization scheme, the flotation comprises sulfur floating and titanium floating, the sulfur floating adopts a primary coarse sweeping flow and a secondary sweeping flow, and the titanium floating adopts a primary coarse sweeping flow, a secondary sweeping flow and a secondary fine sweeping flow.
In the further optimization scheme, the dosage of the sulfuric acid in the sulfur floating process is 500g/t, and the dosage of the No. 2 oil is 60 g/t.
According to a further optimized scheme, the using amount of the collecting agent in the floating titanium is 1800g/h, and the using amount of the regulator is 1200 g/t; in the two refining processes, the addition amount of the first sulfuric acid is 350g/t, and the addition amount of the second sulfuric acid is 200 g/t.
Example 1
(1) Pulse microwave pretreatment: paving the low-grade coated ilmenite in pulse microwave equipment, and performing pulse microwave pretreatment, wherein the pulse frequency is 400Hz, the instantaneous power applied to the material is 40MW, the pulse width is 4 mus, and the irradiation time is 10 s;
(2) grinding: placing the pretreated minerals in a ball mill, wherein the rotating speed of the ball mill is 300r/min, and carrying out ball milling for 4 hours;
(3) magnetic separation: carrying out strong magnetic iron removal on the ground minerals, wherein the magnetic field intensity of the strong magnetic iron removal is 0.5T, the obtained strong magnetic titanium concentrate has 25% of taste and 90% of yield;
(4) flotation: performing flotation on the strong magnetic concentrate, wherein the flotation treatment comprises sulfur flotation and titanium flotation; the sulfur floating adopts a primary coarse sweeping flow and a secondary sweeping flow, and the titanium floating adopts a primary coarse sweeping flow, a secondary sweeping flow and a secondary fine sweeping flow; the dosage of the sulfuric acid is 500g/t and the dosage of the No. 2 oil is 60g/t in the sulfur floating process; the using amount of the collecting agent is 1800g/h and the using amount of the regulator is 1200g/t in the titanium floating process; in the two refining processes, the addition amount of the first sulfuric acid is 350g/t, the addition amount of the second sulfuric acid is 200g/t, and finally the titanium concentrate with the yield of 40.23% and the taste of 51.53% is obtained.
Example 2
(1) Pulse microwave pretreatment: paving the low-grade coated ilmenite in pulse microwave equipment, and performing pulse microwave pretreatment, wherein the pulse frequency is 500Hz, the instantaneous power applied to the material is 60MW, the pulse width is 5 mus, and the irradiation time is 12 s;
(2) grinding: placing the pretreated minerals in a ball mill, wherein the rotating speed of the ball mill is 400r/min, and carrying out ball milling for 5 hours;
(3) magnetic separation: carrying out strong magnetic iron removal on the ground minerals, wherein the magnetic field intensity of the strong magnetic iron removal is 0.7T, so that the obtained strong magnetic titanium concentrate has 27% of taste and 93.6% of yield;
(4) flotation: performing flotation on the strong magnetic concentrate, wherein the flotation treatment comprises sulfur flotation and titanium flotation; the sulfur floating adopts a primary coarse sweeping flow and a secondary sweeping flow, and the titanium floating adopts a primary coarse sweeping flow, a secondary sweeping flow and a secondary fine sweeping flow; the dosage of the sulfuric acid is 500g/t and the dosage of the No. 2 oil is 60g/t in the sulfur floating process; the using amount of the collecting agent is 1800g/h and the using amount of the regulator is 1200g/t in the titanium floating process; in the two refining processes, the addition amount of the sulfuric acid for the first time is 350g/t, the addition amount of the sulfuric acid for the second time is 200g/t, and finally the titanium concentrate with the yield of 42.16% and the taste of 57.96% is obtained.
Example 3
(1) Pulse microwave pretreatment: paving the low-grade coated ilmenite in pulse microwave equipment, and performing pulse microwave pretreatment, wherein the pulse frequency is 550Hz, the instantaneous power applied to the material is 70MW, the pulse width is 7 mus, and the irradiation time is 15 s;
(2) grinding: placing the pretreated minerals in a ball mill, wherein the rotating speed of the ball mill is 500r/min, and carrying out ball milling for 7 h;
(3) magnetic separation: carrying out strong magnetic iron removal on the ground minerals, wherein the magnetic field intensity of the strong magnetic iron removal is 0.9T, so that the obtained strong magnetic titanium concentrate has the taste of 30.42% and the yield of 95%;
(4) flotation: performing flotation on the strong magnetic concentrate, wherein the flotation treatment comprises sulfur flotation and titanium flotation; the sulfur floating adopts a primary coarse sweeping flow and a secondary sweeping flow, and the titanium floating adopts a primary coarse sweeping flow, a secondary sweeping flow and a secondary fine sweeping flow; the dosage of the sulfuric acid is 500g/t and the dosage of the No. 2 oil is 60g/t in the sulfur floating process; the using amount of the collecting agent is 1800g/h and the using amount of the regulator is 1200g/t in the titanium floating process; in the two refining processes, the addition amount of the first sulfuric acid is 350g/t, the addition amount of the second sulfuric acid is 200g/t, and finally the titanium concentrate with the yield of 46.96% and the grade of 58.72% is obtained.
Example 4
(1) Pulse microwave pretreatment: paving the low-grade coated ilmenite in pulse microwave equipment, and performing pulse microwave pretreatment, wherein the pulse frequency is 600Hz, the instantaneous power applied to the material is 80MW, the pulse width is 8 mus, and the irradiation time is 17 s;
(2) grinding: placing the pretreated minerals in a ball mill, wherein the rotating speed of the ball mill is 800r/min, and carrying out ball milling for 7 h;
(3) magnetic separation: carrying out strong magnetic iron removal on the ground minerals, wherein the magnetic field intensity of the strong magnetic iron removal is 1.0T, so that the obtained strong magnetic titanium concentrate has the taste of 35.27% and the yield of 96.8%;
(4) flotation: performing flotation on the strong magnetic concentrate, wherein the flotation treatment comprises sulfur flotation and titanium flotation; the sulfur floating adopts a primary coarse sweeping flow and a secondary sweeping flow, and the titanium floating adopts a primary coarse sweeping flow, a secondary sweeping flow and a secondary fine sweeping flow; the dosage of the sulfuric acid is 500g/t and the dosage of the No. 2 oil is 60g/t in the sulfur floating process; the using amount of the collecting agent is 1800g/h and the using amount of the regulator is 1200g/t in the titanium floating process; in the two refining processes, the addition amount of the first sulfuric acid is 350g/t, the addition amount of the second sulfuric acid is 200g/t, and finally the titanium concentrate with the yield of 47.13% and the taste of 60.07% is obtained.
Example 5
(1) Pulse microwave pretreatment: paving the low-grade coated ilmenite in pulse microwave equipment, and performing pulse microwave pretreatment, wherein the pulse frequency is 700Hz, the instantaneous power applied to the material is 90MW, the pulse width is 10 mus, and the irradiation time is 20 s;
(2) grinding: placing the pretreated minerals in a ball mill, wherein the rotating speed of the ball mill is 700r/min, and carrying out ball milling for 8 hours;
(3) magnetic separation: carrying out strong magnetic iron removal on the ground minerals, wherein the magnetic field intensity of the strong magnetic iron removal is 1.2T, the obtained strong magnetic titanium concentrate has 33% of taste and 96% of yield;
(4) flotation: performing flotation on the strong magnetic concentrate, wherein the flotation treatment comprises sulfur flotation and titanium flotation; the sulfur floating adopts a primary coarse sweeping flow and a secondary sweeping flow, and the titanium floating adopts a primary coarse sweeping flow, a secondary sweeping flow and a secondary fine sweeping flow; the dosage of the sulfuric acid is 500g/t and the dosage of the No. 2 oil is 60g/t in the sulfur floating process; the using amount of the collecting agent is 1800g/h and the using amount of the regulator is 1200g/t in the titanium floating process; in the two refining processes, the addition amount of the first sulfuric acid is 350g/t, the addition amount of the second sulfuric acid is 200g/t, and finally the titanium concentrate with the yield of 48.23% and the taste of 62% is obtained.
In the description of the present invention, it is to be understood that the terms "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, are merely for convenience of description of the present invention, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.

Claims (7)

1. A method for improving the recovery rate of titanium concentrate by pulse microwave pretreatment is characterized by comprising the following steps: the method comprises the following steps:
(1) pulse microwave pretreatment: paving the low-grade coated ilmenite in pulse microwave equipment for pulse microwave pretreatment;
(2) grinding: placing the pretreated minerals in a ball mill;
(3) magnetic separation: carrying out strong magnetic iron removal on the ground minerals to obtain strong magnetic titanium concentrate;
(4) flotation: and carrying out flotation on the strong magnetic concentrate to obtain the titanium concentrate.
2. The pulsed microwave pretreatment for improving the recovery rate of the titanium concentrate according to claim 1, wherein the pulsed microwave pretreatment comprises the following steps: in the pulse microwave pretreatment, the pulse frequency is 400-700Hz, the instantaneous power added on the low-grade coated ilmenite is 40-90MW, the pulse width is 4-10 mus, and the irradiation time is 10-20 s.
3. The pulsed microwave pretreatment for improving the recovery rate of the titanium concentrate according to claim 1, wherein the pulsed microwave pretreatment comprises the following steps: in the ore grinding, the rotating speed of the ball mill is 300-700r/min, and the ball milling is carried out for 4-8 h.
4. The pulsed microwave pretreatment for improving the recovery rate of the titanium concentrate according to claim 1, wherein the pulsed microwave pretreatment comprises the following steps: in the magnetic separation, the magnetic field intensity of the strong magnetic deironing is 0.5-1.2T.
5. The pulsed microwave pretreatment for improving the recovery rate of the titanium concentrate according to claim 1, wherein the pulsed microwave pretreatment comprises the following steps: the flotation comprises sulfur floating and titanium floating, the sulfur floating adopts a primary coarse sweeping flow and a secondary sweeping flow, and the titanium floating adopts a primary coarse sweeping flow, a secondary sweeping flow and a secondary fine sweeping flow.
6. The pulsed microwave pretreatment for improving the recovery rate of the titanium concentrate according to claim 5, wherein the pulsed microwave pretreatment comprises the following steps: the dosage of the sulfuric acid in the sulfur floating process is 500g/t, and the dosage of the No. 2 oil is 60 g/t.
7. The pulsed microwave pretreatment for improving the recovery rate of the titanium concentrate according to claim 5, wherein the pulsed microwave pretreatment comprises the following steps: the using amount of the collecting agent in the floating titanium is 1800g/h, and the using amount of the regulator is 1200 g/t; in the two refining processes, the addition amount of the first sulfuric acid is 350g/t, and the addition amount of the second sulfuric acid is 200 g/t.
CN201911094663.3A 2019-11-11 2019-11-11 Method for improving recovery rate of titanium concentrate through pulse microwave pretreatment Pending CN111054520A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113499855A (en) * 2021-05-27 2021-10-15 中国地质科学院郑州矿产综合利用研究所 Method for improving iron removal effect of glass-phase coal-based waste by adopting microwave pretreatment
CN114985098A (en) * 2021-12-03 2022-09-02 昆明理工大学 Beneficiation and recovery process of micro-fine particle ilmenite

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CN107371290A (en) * 2017-07-12 2017-11-21 刘焕章 A kind of microwave ore heater box
CN107876205A (en) * 2017-11-13 2018-04-06 中钢集团马鞍山矿山研究院有限公司 A kind of beneficiation method that ilmenite is reclaimed from low-grade titaniferous iron tailings
CN109046759A (en) * 2018-09-29 2018-12-21 攀钢集团攀枝花钢铁研究院有限公司 A kind of ilmenite beneficiation method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101553323A (en) * 2006-10-16 2009-10-07 技术资源有限公司 Sorting mined material
CN102319622A (en) * 2011-08-17 2012-01-18 昆明理工大学 Method for improving grade of rutile through microwave pretreatment-magnetic separation combined process
CN104150739A (en) * 2014-08-11 2014-11-19 华东理工常熟研究院有限公司 Method for drying inorganic fine-grained sludge and movable drying system
CN107371290A (en) * 2017-07-12 2017-11-21 刘焕章 A kind of microwave ore heater box
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CN109046759A (en) * 2018-09-29 2018-12-21 攀钢集团攀枝花钢铁研究院有限公司 A kind of ilmenite beneficiation method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113499855A (en) * 2021-05-27 2021-10-15 中国地质科学院郑州矿产综合利用研究所 Method for improving iron removal effect of glass-phase coal-based waste by adopting microwave pretreatment
CN114985098A (en) * 2021-12-03 2022-09-02 昆明理工大学 Beneficiation and recovery process of micro-fine particle ilmenite
CN114985098B (en) * 2021-12-03 2022-11-18 昆明理工大学 Beneficiation and recovery process of micro-fine particle ilmenite

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Application publication date: 20200424