CN114985098A - Beneficiation and recovery process of micro-fine particle ilmenite - Google Patents
Beneficiation and recovery process of micro-fine particle ilmenite Download PDFInfo
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- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000011084 recovery Methods 0.000 title claims abstract description 42
- 239000010419 fine particle Substances 0.000 title claims abstract description 35
- 238000005188 flotation Methods 0.000 claims abstract description 80
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000010936 titanium Substances 0.000 claims abstract description 66
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 66
- 238000000034 method Methods 0.000 claims abstract description 53
- 238000007885 magnetic separation Methods 0.000 claims abstract description 51
- 230000008569 process Effects 0.000 claims abstract description 43
- 239000003814 drug Substances 0.000 claims abstract description 34
- 239000012141 concentrate Substances 0.000 claims abstract description 30
- 238000006477 desulfuration reaction Methods 0.000 claims abstract description 28
- 230000023556 desulfurization Effects 0.000 claims abstract description 28
- 238000005189 flocculation Methods 0.000 claims abstract description 21
- 230000016615 flocculation Effects 0.000 claims abstract description 21
- 238000000227 grinding Methods 0.000 claims abstract description 20
- 239000006185 dispersion Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000006148 magnetic separator Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 3
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 claims abstract description 3
- 241000658379 Manihot esculenta subsp. esculenta Species 0.000 claims abstract description 3
- 229920002472 Starch Polymers 0.000 claims abstract description 3
- 239000011734 sodium Substances 0.000 claims abstract description 3
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 3
- 239000008107 starch Substances 0.000 claims abstract description 3
- 235000019698 starch Nutrition 0.000 claims abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 52
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- 238000007667 floating Methods 0.000 claims description 21
- 239000003153 chemical reaction reagent Substances 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 14
- 239000003784 tall oil Substances 0.000 claims description 14
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 10
- 230000002000 scavenging effect Effects 0.000 claims description 10
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 5
- 230000005611 electricity Effects 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000003311 flocculating effect Effects 0.000 abstract description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 21
- 239000011707 mineral Substances 0.000 description 21
- 238000010438 heat treatment Methods 0.000 description 11
- 239000002245 particle Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 238000000926 separation method Methods 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- IRDQNLLVRXMERV-UHFFFAOYSA-N CCCC[Na] Chemical compound CCCC[Na] IRDQNLLVRXMERV-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000004088 foaming agent Substances 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000012991 xanthate Substances 0.000 description 5
- 229910001773 titanium mineral Inorganic materials 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000005065 mining Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010494 dissociation reaction Methods 0.000 description 2
- 230000005593 dissociations Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000008396 flotation agent Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229910052611 pyroxene Inorganic materials 0.000 description 2
- HBROZNQEVUILML-UHFFFAOYSA-N salicylhydroxamic acid Chemical compound ONC(=O)C1=CC=CC=C1O HBROZNQEVUILML-UHFFFAOYSA-N 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- 229910021532 Calcite Inorganic materials 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 241000131774 Tectona Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- 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
- B03B9/00—General arrangement of separating plant, e.g. flow sheets
-
- 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
- B03B1/00—Conditioning for facilitating separation by altering physical properties of the matter to be treated
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/52—Mechanical processing of waste for the recovery of materials, e.g. crushing, shredding, separation or disassembly
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a beneficiation and recovery process of micro-fine ilmenite, which comprises the following steps: the method comprises the following steps of selective dispersing, flocculating and magnetic separation after fine grinding: further finely grinding the fine-particle ilmenite, mixing and stirring the fine-particle ilmenite with a medicament FX-3 to realize selective dispersion flocculation, and then feeding the mixture into a high-gradient strong magnetic separator for magnetic separation under the condition of high frequency of washing; the dosage of FX-3 is not less than 500g/(t raw ore), and the weight ratio of the FX-3 to the raw ore is as follows: 20 to 35 percent of modified cassava starch, 10 to 25 percent of carboxymethyl cellulose and 40 to 70 percent of sodium fluosilicate. The microwave short-flow flotation after desulfurization: and performing conventional flotation and desulfurization on the magnetic concentrate, performing microwave treatment on the desulfurization tailing by using equipment MT-2, and then performing titanium flotation with low medicament dosage and short flow. MT-2 is independently developed, the working power is 2500W-3600W, and the working frequency does not exceed 750 MHz. The new process of the invention can effectively realize the recovery of the fine ilmenite, and has the advantages of small medicament dosage, low cost, short flow and convenient operation and implementation.
Description
Technical Field
The invention belongs to the field of titanium beneficiation and comprehensive resource recovery, and particularly relates to a beneficiation and recovery process of fine-particle ilmenite, in particular to a process of selective dispersion flocculation magnetic separation after fine grinding and microwave short-flow flotation after desulfurization.
Background
The source of the micro-fine ilmenite is generally iron tailings, and the current process for mineral separation and recovery of the micro-fine ilmenite is mainly a strong magnetic-flotation process. With the continuous development of flotation agents in recent years, novel flotation agents such as R-2, ROB, RST, ZY, XT, TAO series, MOH series and MOS are formed, and the grade and the yield of titanium concentrate are improved to a certain extent.
However, as the mining depth of a mine increases, the properties of the accompanying ore also vary greatly. In the Panxi region for example, the olivine component in the ore is gradually increased, so that the ilmenite in most mines is changed from the original pyroxene type to the pyroxene type, and the embedded part granularity of useful minerals is gradually reduced, which is most representative in the North Hongge mine area. The ore properties are greatly changed, and the ore dressing recovery difficulty is increased. For example, Tectona tetrapanacis, TiO in two-stage high intensity magnetic separation tailings 2 The grade is about 5 percent approximately, the yield of the micro-fine particles (-38 mu m) reaches 61 percent, and the particle size fraction TiO 2 The distribution rate even reaches 80 percent, and the part of the fine-particle ilmenite enters tailings, thereby seriously restricting the improvement of the titanium recovery rate.
For the beneficiation of ilmenite, there is a problem that the recovery rate is mainly too low. Research and analysis have shown that titanium is mainly lost in the fine fraction (fine ilmenite is difficult to recover and runs out severely). In industrial processes, TiO in fine-grained ilmenite 2 Recovery rate is lower thanIlmenite with a size fraction of 50%, especially in the range of-19 μm, is even less efficient separation and enrichment process. At present, the ilmenite with the particle size fraction of-19 mu m is mainly treated by adopting a tailing pond stockpiling method, so that a large amount of titanium resources are lost and wasted over time. Therefore, the improvement of the recovery rate of titanium is essentially to strengthen the recovery of fine ilmenite.
The aging team performs the process flow of dry preselection, ore grinding, low intensity magnetic separation, strong magnetic separation and flotation on dry iron tailings with iron grade of 15.20 percent and titanium grade of 9.65 percent, and the grade and recovery rate of the final titanium concentrate are 45.29 percent and 45.34 percent.
The actual production experiment of the ilmenite used by the Yongbang team is carried out, and the process comprises the steps of firstly discarding the tail of the ilmenite by using a SLon-1500 magnetic separator to obtain rough concentrate, wherein TiO is used as the rough concentrate 2 The grade of the product is increased from 11.03 percent to 21.23 percent, and the grade of the product is TiO 2 The recovery was 76.24%; the flotation adopts a process flow of rough four fine scans, and the used flotation reagents comprise: collecting agent MOS, inhibitor carboxymethyl cellulose and water glass to obtain titanium concentrate, TiO 2 The grade is 47.31%, and the recovery rate reaches 61.65%.
The Xie nationality team adopts ROB as a flotation collector to perform mineral separation on the fine-particle ilmenite in the Panzhihua region, the-43 mu m particle size fraction accounts for 61.2-64.1%, and titanium concentrate is obtained after the flotation is finished, wherein TiO is 2 Grade is 48 percent, and recovery rate is 65 percent.
The Deng ice team performs multi-component chemical analysis and mineral identification on the ore taken from the vanadium titano-magnetite in the Panxi area, and based on the multi-component chemical analysis and the mineral identification, the high-intensity magnetic separation is adopted to pre-enrich the titanium mineral, TiO mineral 2 The grade of the titanium ore is increased by 7.35 percent on the original basis, then the rougher concentrate is floated, and the titanium ore concentrate is finally obtained by adopting the flow of 'once rougher flotation, four times of cleaner flotation and once scavenging', wherein TiO is 2 The grade and the operation recovery rate respectively reach 47.78 percent and 61.25 percent.
It is generally considered that magnetic separation depends on equipment and flotation depends on chemicals, so that the research focus of conventional magnetic separation is mainly focused on equipment aspects, such as a pulsating high gradient magnetic separator (Ganzhou Jinhuan, Guangzhou institute, Shandong Huate and the like), and the research focus of flotation is focused on chemicals aspects, such as MOH, MOS, salicylhydroxamic acid and the like. At present, the conventional strong magnetic-flotation process and research results tend to be unified, the grade and the recovery rate of titanium concentrate are low, particularly the recovery rate is even lower than 40% in partial separation plants (magnetic separation is 50-60%, flotation is about 50%); and the process is long (usually more than 4 stages of fine separation are needed), the medicament consumption is high (acid environment flotation, the utilization efficiency of collecting agents is low), and the medicament cost is high (salicylhydroxamic acid and the like are expensive). Therefore, in order to fully and effectively utilize the resources of the micro-fine ilmenite, a new process for efficiently beneficiation and recovery of the micro-fine ilmenite is researched and developed on the basis of a conventional beneficiation process, and a beneficiation process flow which is technically and economically reasonable is found, which is undoubtedly significant.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a beneficiation and recovery process of fine-particle ilmenite, in particular to a process of selective dispersion flocculation magnetic separation after fine grinding and microwave short-flow flotation after desulfurization. The process can effectively realize the recovery of the fine ilmenite, and has the advantages of small medicament dosage, low cost, short flow and convenient operation and implementation.
In order to solve the technical problems, the invention adopts the technical scheme that:
the beneficiation and recovery process of the fine particle grade ilmenite comprises the following specific steps:
s1 selective dispersing flocculation magnetic separation after fine grinding: further finely grinding the fine-particle ilmenite, mixing and stirring the fine-particle ilmenite with a medicament FX-3, realizing selective dispersion flocculation, feeding the mixture into a high-gradient strong magnetic separator, and carrying out magnetic separation under the condition of high frequency of washing;
and (3) microwave short-flow flotation after S2 desulfurization: and performing conventional flotation and desulfurization on the magnetic concentrate, performing microwave treatment on the desulfurization tailing by using equipment MT-2, and performing short-flow titanium flotation according to low medicament dosage to obtain the titanium concentrate.
Further, TiO in the fine-particle ilmenite raw ore 2 The content of (A) is 6% -8%.
Further, the fine ilmenite is further ground to a fineness of more than 85% in an occupancy of-25 μm.
Further, adjusting the concentration of the ore pulp of the fine grinding material to be between 15 and 35 percent; then, mixing and stirring the ore pulp and the reagent FX-3 to realize selective dispersion flocculation; the stirring time is required to be not less than 10min, and dispersed flocculated ore pulp is prepared; the main components of the selective dispersion flocculation reagent FX-3 are as follows: modified cassava starch (20-35 wt%), carboxymethyl cellulose (10-25 wt%) and sodium fluosilicate (40-70 wt%); wherein the dosage of the selective dispersion flocculation medicament FX-3 is required to be not less than 500g/(t of raw ore).
Furthermore, the high gradient magnetic separation must be carried out under the condition of high frequency of impact, and the frequency of impact is not less than 260 times/min. The number of magnetic separation sections is determined according to the properties of the micro-fine particle ilmenite, the grade requirement of flotation feeding and the like, the requirements can be met by two-section open-circuit magnetic separation, and high-gradient magnetic separation concentrates of the first section and the second section can be combined to be used as final concentrates; the magnetic field intensity of the first-stage high-gradient magnetic separation is 0.5T-1.2T, and the magnetic field intensity of the second-stage high-gradient magnetic separation is 0.6T-1.3T.
Further, the flotation reagents selected in the conventional desulfurization treatment process include: regulator sulfuric acid, collecting agent butyl sodium xanthate and foaming agent 2 # An oil; wherein, the dosage of the regulator sulfuric acid is 1100-1300 g/(t raw ore), the dosage of the collector butyl sodium xanthate is 200-400 g/(t raw ore), and the foaming agent 2 # The amount of the oil is 35-45 g/(t of raw ore).
Further, after the desulfurization tailings are obtained, the method further comprises the following steps: and carrying out microwave treatment on the desulfurization tailings to obtain a titanium flotation raw material. Microwave equipment MT-2 adopted by the microwave treatment; the working power of the microwave equipment MT-2 is required to be 2500W-3600W, and the working frequency is required not to exceed 750 MHz. Microwave equipment MT-2 includes microwave barrel body, microwave generator 1, microwave transducer 2, controller, be equipped with ore pulp entry 9 in the middle of the top surface of microwave barrel body, be equipped with water inlet 8 on the lateral wall of top, the bottom is equipped with ore pulp export 10, be equipped with a plurality of swash plates in the microwave barrel body, swash plate one end is connected on the bucket wall, and the other end inclines to bucket inner lower part, and cross arrangement about a plurality of swash plates forms Z type passageway, microwave ring energy ware 2 is installed in swash plate and bucket wall junction, and microwave generator 1 installs on the back of swash plate, microwave generator 1 is connected with microwave transducer 2 electricity, microwave transducer 2 is connected with the controller electricity.
Furthermore, on the premise that the microwave treatment is carried out on the titanium floating raw material by the process, the short-flow titanium floating can be realized, and the requirement can be met by reducing the number of the fine selection stages of the conventional flotation to be not more than 2 stages; the treatment of the titanium flotation raw material also comprises a first-stage roughing and a first-stage scavenging, wherein the scavenged tailings are discharged as final tailings.
Furthermore, on the premise that the process carries out microwave treatment on the titanium floating raw material, the titanium floating with low medicament dosage can be realized. Wherein, the medicament selected by rough selection comprises: regulating agent sulfuric acid and collecting agent tall oil, wherein the dosage of the sulfuric acid is only 500-650 g/(t raw ore), and the dosage of the tall oil is only 500-700 g/(t raw ore); selecting a selected medicament as a regulator sulfuric acid, wherein the dosage of the sulfuric acid is required to be 150-200 g/(t of raw ore); the medicament selected for scavenging comprises: the modifier sulfuric acid and the collector tall oil are used, the dosage of the sulfuric acid is only 100-150 g/(t raw ore), and the dosage of the tall oil is only 250-350 g/(t raw ore).
Further, in the titanium floating process, the pH value of the ore pulp is required to be 5.0-6.5.
After the technical scheme is adopted, compared with the prior art, the invention has the following beneficial effects.
1. In the fine-particle ilmenite, a large amount of slime generated in the mining and grinding processes is contained, and if the fine-particle ilmenite directly enters strong magnetic separation, the fine-particle ilmenite is very easy to lose due to the fact that the separation force acting on mineral particles is very low due to the fact that a large amount of secondary slime is contained, and finally the grade and the recovery rate of magnetic separation concentrate are influenced. According to the property characteristics of the fine-particle ilmenite, the research origin is changed, and the conventional strong magnetic-flotation process is optimized and improved.
The conventional magnetic separation has the problems of low recovery rate and low pre-enrichment degree, and the process is inspired from flotation reagents and introduces the reagents into the magnetic separation. The existing micro-fine ilmenite is generally not further finely ground, and the new process needs to finely grind the micro-fine ilmenite, so that the micro-fine ilmenite is fully dissociated, micro-fine titanium minerals and gangue particles are stably dispersed in ore pulp through a self-compounded selective dispersing flocculating agent FX-3, and the micro-fine titanium minerals and the agent FX-3 interact to form unstable mineral particles. The mineral particles are gradually transformed into floccules through the bridging action and form more stable floccules under the continuous action of mechanical stirring, so that the apparent size of the target mineral particles is increased, and the strong magnetic separation effect and the separation force acting on the titanium mineral particles are effectively improved.
On the basis of conventional flotation, equipment MT-2 is introduced to carry out microwave heating treatment, so that the monomer dissociation degree of useful minerals is improved, the flotation performance of fine-particle ilmenite is improved, and titanium floatation with low medicament consumption and short flow is realized.
2. In the face of the problem of low pre-enrichment degree, higher frequency of impact can be controlled during magnetic separation, the grade of magnetic separation concentrate can be effectively improved while higher recovery rate is ensured, so that more qualified feed is provided for subsequent flotation, the burden of subsequent flotation is greatly reduced, the number of stages of fine selection during flotation can be effectively reduced, the using amount of flotation reagents is reduced, and the recovery rate of flotation operation is improved.
3. Because the required microwave treatment equipment is lacked in the field of mineral separation at present, after a large number of relevant documents are consulted and professional personnel are consulted, the suggestions of all parties are combined, the microwave treatment equipment MT-2 suitable for the flotation of the fine ilmenite is finally designed, and the application of the microwave treatment equipment MT-2 in the flotation is realized by adjusting equipment parameters.
The existing flotation process has long flow, more than 4 stages of fine selection are often needed, and the dosage of the medicament is large. The invention adds microwave processing equipment MT-2 on the basis of the conventional flotation process and medicament. The microwave has the characteristics of shorter wavelength, higher frequency, penetrating through an ionized layer and the like, the heat of the traditional heating is conducted from the outside to the inside, and the microwave is different from the traditional heating mode and has the principle of volume heating caused by the internal molecular polarization of the material in a microwave field. Along with the alternating change of the microwave electromagnetic field, the polarized molecules in the substance also generate high-frequency oscillation, and further generate heat. In addition, the microwave heating has the characteristics of integral heating, selective heating, instant heating, chemical reaction strengthening, process energy consumption reduction, safety, environmental protection and the like. The microwave treatment can effectively improve the flotation performance of the micro-fine ilmenite and improve the titanium flotation effect.
The gangue minerals in the ore are mainly quartz and calcite. The rate of temperature rise for gangue minerals is low, while the rate of temperature rise for useful minerals is relatively high. Thus, a very significant local temperature difference is formed between the gangue minerals and the useful minerals, thereby generating thermal stress therebetween. When the thermal stress reaches a certain level, cracks can occur at the mineral interface. The generation of cracks can effectively promote the monomer dissociation of the useful minerals, improve the specific surface area of the useful minerals and have important significance for improving the recovery rate of the titanium separation.
In the past, microwave flotation has two problems, namely how to intervene in a flotation link and how to avoid the evaporation of a large amount of water in ore pulp during the microwave heating action. The invention effectively solves the problem through microwave processing equipment MT-2 independently invented by Kunming technology university, adopts a multi-site, low-frequency and low-power mode, and enables ore pulp to be heated by microwaves in a flowing environment, thereby effectively avoiding the evaporation of a large amount of ore pulp in the heating process and achieving ideal effect on the action of mineral particles. From the perspective of the flotation process, the appropriate temperature rise is also beneficial to the subsequent flotation process flow.
The flotation process can be reduced after microwave heating treatment, the number of fine selection sections can be reduced, the number of fine selection sections of conventional flotation can be reduced to be not more than 2 sections, and the medicament dosage of the original collecting agent and the original regulating agent is obviously reduced through microwave treatment.
Based on the description of the aspects, the novel process can effectively realize the beneficiation recovery of the micro-fine ilmenite, particularly the TiO-containing micro-fine ilmenite 2 Under the condition of less than 8 percent, compared with the prior and conventional strong magnetic-flotation process, the titanium grade and the titanium recovery rate of the final concentrate are improved. The new process of the invention has small dosage and low costThe method has the advantages of low cost, short flow and convenient operation and implementation.
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention to its proper form. It is obvious that the drawings in the following description are only some embodiments, and that for a person skilled in the art, other drawings can be derived from them without inventive effort. In the drawings:
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a schematic diagram of an apparatus for microwave processing equipment MT-2;
in the figure: 1-microwave sounder; 2-a micro-wave transducer; 3-a security system; 4-frequency, power divider; 6-a power supply system; 7-a power switch; 8-water inlet; 9-a pulp inlet; 10-slurry outlet.
It should be noted that the drawings and the description are not intended to limit the scope of the inventive concept in any way, but to illustrate it by a person skilled in the art with reference to specific embodiments.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and the following embodiments are used for illustrating the present invention and are not intended to limit the scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1:
the ilmenite raw material is taken from the tailings pond of Panzhihuaxiou river ore and TiO 2 The content of the ilmenite is only 6.59 percent, the particle size distribution of the ilmenite is relatively dispersed, and the ilmenite belongs to low-grade and micro-fine particle refractory ilmenite tailings.
The process flow shown in figure 1 is adopted, and specifically comprises the following steps:
s1 selective dispersing flocculation magnetic separation after fine grinding: further finely grinding the fine-particle ilmenite, mixing and stirring the fine-particle ilmenite with a medicament FX-3, realizing selective dispersion flocculation, feeding the mixture into a high-gradient strong magnetic separator, and carrying out magnetic separation under the condition of high frequency of washing;
and (3) microwave short-flow flotation after S2 desulfurization: and performing conventional flotation and desulfurization on the magnetic concentrate, performing microwave treatment on the desulfurization tailing by using equipment MT-2, and performing short-flow titanium flotation according to low medicament dosage to obtain the titanium concentrate.
Wherein the occupancy of-25 μm fineness is 88%.
Wherein, the concentration of the ore pulp of the fine grinding material is adjusted to 20 percent; then, fully stirring the ore pulp and the reagent FX-3 for 15min at the rotating speed of 600r/min to prepare dispersed flocculating ore pulp; wherein the dosage of the selective dispersion flocculation reagent FX-3 is 800g/(t raw ore).
Wherein the number of impact times in the strong magnetic separation process is 300 times/min, and the method comprises two-stage open-circuit magnetic separation, wherein the magnetic field intensity of the I-stage high-gradient magnetic separation is 1.0T, and the magnetic field intensity of the II-stage high-gradient magnetic separation is 1.2T.
Wherein, the medicament system in the flotation desulfurization process is as follows: 1200g/(t raw ore) of regulator sulfuric acid,Collecting agent butyl sodium xanthate 300g/(t raw ore) and foaming agent 2 # Oil 40g/(t raw ore).
After obtaining the desulfurization tailings, performing microwave treatment on the desulfurization tailings to obtain a titanium flotation raw material; the microwave treatment adopts microwave equipment MT-2; the working power of the microwave equipment MT-2 is 2600W, and the working frequency is 700 MHz. Its structure of microwave equipment MT-2 here refers to attached drawing 2 and shows, MT-2 includes microwave barrel body, microwave generator 1, microwave transducer 2, controller, be equipped with ore pulp entry 9 in the middle of the top surface of microwave barrel body, be equipped with water inlet 8 on the lateral wall of top, the bottom is equipped with ore pulp export 10, be equipped with a plurality of swash plates in the microwave barrel body, swash plate one end is connected on the bucket wall, and the other end inclines to the lower part in the bucket, and the cross arrangement is controlled to a plurality of swash plates, forms Z type passageway, microwave ring energy ware 2 is installed in swash plate and bucket wall junction, and microwave generator 1 installs on the back of swash plate, microwave generator 1 is connected with microwave transducer 2 electricity, and each swash plate all corresponds a microwave transducer 2, and each microwave transducer 2 all corresponds a microwave generator 1. The micro-wave transducer 2 is electrically connected with a controller, the controller comprises a safety system 3, a frequency power divider 4, a power supply system 6 and a power switch 7, the structure of the controller part is the prior art, namely the control system part, in the example, the controller is applied to control the micro-wave transducer 2, the micro-wave transducer 2 is a device which can convert high-frequency electric energy into mechanical energy, the piezoelectric effect of materials converts electric signals into mechanical vibration, and the micro-wave transducer is an energy conversion device which converts input electric power into mechanical power (namely microwave) and then transmits the mechanical power, and consumes a small part of power. By the arrangement of the microwave transducer 2, the microwave effect can be enhanced.
After the titanium floating raw material is obtained, the pulp concentration is adjusted to 35% by a stirring barrel at the rotating speed of 550 r/min.
Wherein, the titanium flotation comprises 'one-stage roughing and two-stage fine selection' of the titanium flotation raw material (after the microwave treatment of the desulfurization tailings); in addition, the method also comprises a step of scavenging the rougher tailings, wherein the scavenged tailings are discharged as final tailings.
Wherein, the medicament system selected in the roughing operation of the floating titanium comprises the following components: the dosage of the regulator sulfuric acid is 600g/(t raw ore), and the dosage of the collector tall oil is 600g/(t raw ore); the dosage of the regulator sulfuric acid used in the two-stage concentration operation in the titanium flotation is 200g/(t of raw ore); the dosage of sulfuric acid used as a scavenging operation regulator in the titanium flotation is 150g/(t of raw ore), and the dosage of tall oil used as a collector is 300g/(t of raw ore). The pulp pH was adjusted to 6.0.
TiO is finally obtained 2 Grade 49.31% TiO 2 The recovery rate of the titanium concentrate is 70.02 percent.
Example 2:
the ilmenite raw material is taken from the tailing pond of the Panzhihua HongGenan mining area and TiO 2 The content of the tailings is only 7.01 percent, and the tailings belong to low-grade and micro-fine particle refractory ilmenite type tailings.
The process flow shown in figure 1 is adopted, and specifically comprises the following steps:
s1 selective dispersing flocculation magnetic separation after fine grinding: further finely grinding the fine-particle ilmenite, mixing and stirring the fine-particle ilmenite with a medicament FX-3 to realize selective dispersion flocculation, and then feeding the mixture into a high-gradient strong magnetic separator for magnetic separation under the condition of high frequency of washing;
s2 microwave short-flow flotation after desulfurization: and performing conventional flotation and desulfurization on the magnetic concentrate, performing microwave treatment on the desulfurization tailing by using equipment MT-2, and performing short-flow titanium flotation according to a conventional medicament system to obtain the titanium concentrate.
Wherein the occupancy of-25 μm fineness is 95%.
Wherein, the concentration of the ore pulp of the fine grinding material is adjusted to 20 percent; then, fully stirring the ore pulp and the reagent FX-3 for 10min at the rotating speed of 700r/min to prepare dispersed flocculating ore pulp; wherein the dosage of the selective dispersion flocculation medicament FX-3 is 600g/(t raw ore).
Wherein, the number of times of impact in the strong magnetic separation process is 280 times/min, and the method also comprises two sections of open-circuit magnetic separation, wherein the magnetic field intensity of the I section of high-gradient magnetic separation is 0.9T, and the magnetic field intensity of the II section of high-gradient magnetic separation is 1.1T.
Wherein, the reagent system of the flotation desulphurization is as follows: 1100g of regulating agent sulfuric acid/(t raw ore), 250g of collecting agent butyl sodium xanthate/(t raw ore) and 2 g of foaming agent # Oil 40g/(t raw ore).
After the desulfurized tailings are obtained, performing microwave treatment on the desulfurized tailings to obtain floating materials; the microwave equipment MT-2 used for the above microwave processing is the same as that in embodiment 1, and is not described herein again; the working power of the microwave equipment MT-2 is 3000W, and the working frequency is 600 MHz.
After the floating material is obtained, the concentration of the ore pulp is adjusted to 30% through a stirring barrel at the rotating speed of 500 r/min.
Wherein, the titanium floating comprises 'first-stage roughing and second-stage concentrating' of the titanium floating raw material; in addition, the method also comprises a step of scavenging the rougher tailings, wherein the scavenged tailings are discharged as final tailings.
Wherein, the medicament system selected in the roughing operation of the floating titanium comprises the following components: the dosage of the regulator sulfuric acid is 600g/(t raw ore), and the dosage of the collector tall oil is 600g/(t raw ore); the dosage of the regulator sulfuric acid used in the two-stage concentration operation in the titanium flotation is 200g/(t of raw ore); the dosage of sulfuric acid used as a scavenging operation regulator in the titanium flotation is 150g/(t of raw ore), and the dosage of tall oil used as a collecting agent is 300g/(t of raw ore). The pulp pH was adjusted to 6.0.
TiO is finally obtained 2 Grade 50.72% TiO 2 The recovery rate of the titanium concentrate is 68.95 percent.
Example 3:
the ilmenite raw material is taken from Kun steel group Rogowski tailings pond and TiO 2 The content of the tailings is only 6.45 percent, and the tailings also belong to low-grade and micro-fine particle refractory ilmenite tailings.
The process flow shown in figure 1 is adopted, and specifically comprises the following steps:
s1 selective dispersing flocculation magnetic separation after fine grinding: further finely grinding the fine-particle ilmenite, mixing and stirring the fine-particle ilmenite with a medicament FX-3, realizing selective dispersion flocculation, feeding the mixture into a high-gradient strong magnetic separator, and carrying out magnetic separation under the condition of high frequency of washing;
and (3) microwave short-flow flotation after S2 desulfurization: and performing conventional flotation and desulfurization on the magnetic concentrate, performing microwave treatment on the desulfurization tailing by using equipment MT-2, and performing short-flow titanium flotation according to a conventional medicament system to obtain the titanium concentrate.
Wherein the occupancy of-25 μm fineness is 90%.
Wherein, the concentration of the ore pulp of the fine grinding material is adjusted to 20 percent; then, fully stirring the ore pulp and the reagent FX-3 for 15min at the rotating speed of 650r/min to prepare dispersed flocculating ore pulp; wherein the dosage of the selective dispersion flocculation medicament FX-3 is 750g/(t raw ore).
Wherein, the number of times of impact in the strong magnetic separation process is 300 times/min, and the method also comprises two sections of open-circuit magnetic separation, wherein the magnetic field intensity of the I section of high-gradient magnetic separation is 1.0T, and the magnetic field intensity of the II section of high-gradient magnetic separation is 1.2T.
Wherein, the reagent system in the flotation desulfurization process is as follows: 1100g/(t crude ore) of regulating agent sulfuric acid, 200g/(t crude ore) of collecting agent butyl sodium xanthate and 2 g of foaming agent # Oil 40g/(t run).
After the desulfurized tailings are obtained, performing microwave treatment on the desulfurized tailings to obtain floating materials; the microwave equipment MT-2 used for the microwave processing is the same as that in embodiment 1, and is not described herein again; the working power of the microwave equipment MT-2 is 3300W, and the working frequency is 650 MHz.
After the floating material is obtained, the concentration of the ore pulp is adjusted to 35% through a stirring barrel at the rotating speed of 600 r/min.
Wherein, the floating titanium comprises 'one-stage roughing and two-stage concentration' of the floating titanium raw material; in addition, the method also comprises a step of scavenging the rougher tailings, wherein the scavenged tailings are discharged as final tailings.
Wherein, the medicament system selected in the roughing operation of the floating titanium comprises the following components: the dosage of the regulator sulfuric acid is 650g/(t raw ore), and the dosage of the collector tall oil is 600g/(t raw ore); the dosage of the regulator sulfuric acid used in the two-stage concentration operation in the titanium flotation is 200g/(t of raw ore); the dosage of sulfuric acid used as a scavenging operation regulator in the titanium flotation is 150g/(t of raw ore), and the dosage of tall oil used as a collecting agent is 300g/(t of raw ore). The pulp pH was adjusted to 5.5.
TiO can be finally obtained 2 Grade 50.03%, TiO 2 The recovery rate of the titanium concentrate is 69.23 percent.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. The beneficiation and recovery process of the micro-fine ilmenite is characterized by comprising the following steps of:
s1 selective dispersing flocculation magnetic separation after fine grinding: further finely grinding the fine-particle ilmenite, mixing and stirring the fine-particle ilmenite with a medicament FX-3, realizing selective dispersion flocculation, feeding the mixture into a high-gradient strong magnetic separator, and carrying out magnetic separation under the condition of high frequency of washing;
s2 microwave short-flow flotation after desulfurization: and performing conventional flotation and desulfurization on the magnetic concentrate, performing microwave treatment on the desulfurization tailing by using equipment MT-2, and performing short-flow titanium flotation according to low medicament dosage to obtain the titanium concentrate.
2. The beneficiation recovery process of fine ilmenite according to claim 1, wherein the fine ilmenite raw ore is TiO 2 The content of (A) is 6% -8%.
3. The beneficiation and recovery process of fine ilmenite according to claim 1, characterized in that the fine ilmenite is further finely ground, and the fineness of the finely ground product is controlled to be more than 85% in-25 μm occupancy.
4. The beneficiation and recovery process for fine particle ilmenite according to claim 1, characterized in that the selective dispersion flocculation reagent FX-3 comprises the following components in percentage by mass: 20 to 35 percent of modified cassava starch, 10 to 25 percent of carboxymethyl cellulose and 40 to 70 percent of sodium fluosilicate; wherein the dosage of the selective dispersion flocculation medicament FX-3 is not less than 500g/(t of raw ore); the agent FX-3 and the ore pulp are mixed and stirred, the concentration of the ore pulp needs to be adjusted to be 15% -35%, and the stirring action time is not less than 10 min.
5. The beneficiation and recovery process of fine ilmenite according to claim 1, wherein the high gradient magnetic separation must be performed under a high frequency of stroke condition, which requires not less than 260 times/min. The number of the magnetic separation sections is determined according to the properties of the micro-fine particle ilmenite, the grade requirement of flotation feeding and the like, the requirements can be met by two-section open-circuit magnetic separation, and high-gradient magnetic concentrate ores in the first section and the second section can be combined to be used as final concentrate; the magnetic field intensity of the I-section high-gradient magnetic separation is 0.5T-1.2T, and the magnetic field intensity of the II-section high-gradient magnetic separation is 0.6T-1.3T.
6. The beneficiation and recovery process for the fine particle ilmenite according to claim 1, wherein the working power of microwave equipment in microwave treatment is 2500-3600W, and the working frequency is not more than 750 MHz; microwave equipment is MT-2, and MT-2 includes microwave barrel body, microwave generator 1, microwave transducer 2, controller, be equipped with ore pulp entry 9 in the middle of the top surface of microwave barrel body, be equipped with water inlet 8 on the lateral wall of top, the bottom is equipped with ore pulp export 10, be equipped with a plurality of swash plates in the microwave barrel body, swash plate one end is connected on the bucket wall, and the other end inclines to bucket inner lower part, and cross arrangement forms Z type passageway about a plurality of swash plates, microwave ring energy ware 2 is installed in swash plate and bucket wall junction, and microwave generator 1 installs on the back of swash plate, microwave generator 1 is connected with microwave transducer 2 electricity, microwave transducer 2 is connected with the controller electricity.
7. The beneficiation and recovery process for fine particle ilmenite of claim 1, wherein the short-flow titanium flotation can reduce the number of the fine concentration operation stages of the titanium flotation to not more than 2 stages on the premise of performing microwave treatment on the titanium flotation raw material.
8. The beneficiation and recovery process for the fine particle ilmenite of claim 1, wherein the amount of the agent used for floating the titanium is significantly reduced compared with the conventional titanium floating process due to the microwave treatment of the raw material for floating the titanium, which is specifically as follows: the medicament selected by the titanium flotation roughing operation comprises regulating agent sulfuric acid and collecting agent tall oil; the dosage of the regulator sulfuric acid is only 500-650 g/(t raw ore), and the dosage of the collector tall oil is only 500-700 g/(t raw ore); the selected medicament for the floating titanium fine selection operation comprises regulator sulfuric acid; the dosage of the regulator sulfuric acid is 150-200 g/(t raw ore); the flotation reagents selected for titanium flotation scavenging operation comprise regulating agent sulfuric acid and collecting agent tall oil; the dosage of the regulator sulfuric acid is only 100-150 g/(t raw ore), and the dosage of the collector tall oil is only 250-350 g/(t raw ore); in addition, in the titanium flotation process, the pH value of the ore pulp is required to be 5.0-6.5.
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