CN110882830A - Weathered niobium ore beneficiation method - Google Patents
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Abstract
The invention discloses a beneficiation method of weathered niobium ores. The beneficiation method of weathered niobium ores comprises the following steps: grinding raw ores, reselecting a product after grinding to obtain reselected tailings and reselected rough concentrates, carrying out magnetic separation on the reselected rough concentrates in a low-intensity magnetic separator to obtain iron concentrates and low-intensity magnetic tailings, concentrating, roughing, primary scavenging and secondary scavenging the low-intensity magnetic tailings, concentrating to obtain phosphorus concentrates and floating phosphorus tailings, concentrating, roughing, primary scavenging and secondary scavenging the floating phosphorus tailings, and concentrating to obtain floating niobium concentrates and floating niobium tailings. The beneficiation method combines the special properties of weathered niobium ores, adopts the process of combining gravity separation, magnetic separation and flotation, improves the separation and recovery effects of niobium minerals, phosphorus minerals, iron minerals and gangue minerals, obtains niobium concentrate, iron concentrate and phosphorus concentrate products, effectively recovers iron and phosphorus while realizing niobium recovery, and realizes comprehensive recovery and utilization of mineral resources.
Description
Technical Field
The invention relates to the technical field of beneficiation and recovery, and particularly relates to a beneficiation method of weathered niobium ores.
Background
Niobium is a rare refractory metal and is widely applied to the fields of steel, aerospace and the like. China is a typical niobium-poor country, and more than 90% of niobium resources are imported. Over 90% of the global niobium supply is produced from virgin pyrochlore deposits. The weathered niobium deposit resource reserves are huge and widely distributed in African regions, but because the resources are seriously weathered, have more micro-particles, serious iron pollution and extremely difficult to recover, the weathered niobium deposit resources are lack of reasonable technology to develop at present, so the weathered niobium deposit resources are in an undeveloped dull state for a long time.
Urghuaxi et al (mineral dressing experimental research of certain roasted greenstone ore) [ J]275-278. material research and application 2015(04), aiming at that the niobium mineral in a certain ore is mainly pyrochlore, combining the properties of the ore, after desliming and removing the ferromagnetic mineral and the zirconite, the ore is slurried by sulfuric acid, modified water glass, lead nitrate and OA are used as regulators, chelating agent GYX is used as a collector to float and recover the pyrochlore, and Nb is subjected to flotation2O5Feeding ore with the grade of 0.26 percent, and obtaining Nb by closed-loop test2O5The grade of the niobium concentrate is 27.93%, the operation recovery rate is 86.97%, the total recovery rate of niobium is 79.43%, and the effective separation of pyrochlore and gangue minerals is realized. The object of the study was a primary niobium zirconium ore,pyrochlore in the ore has a relatively complete crystal form, is in a poly-shape of an octahedron and a rhombic dodecahedron, is mostly in a self-shaped crystal embedded in mineral such as albite, nepheline and the like, is complete in crystal, has good floatability, and is beneficial to flotation recovery. The tailings of the zircon separation are the primary niobium-zirconium ore, but not the weathered niobium ore, and the specific causes of the agents used in the method are not disclosed. BISS et al (pyrochlore beneficiation of Niobec) concentrating mills) [ J]And comprehensive utilization of mineral products [ J]1983(02) 97-99. the technological process of Nidohbek concentrating mill is mainly described in the text, mainly including: the process flow of crushing and grinding the ore to the size of the dissociation of the useful minerals, desliming, carbonate flotation and re-desliming, magnetic separation, pyrochlore flotation and two stages of pyrite flotation with the final concentrate leaching therebetween is rather complicated. The ore is treated by newly mined carbonic acid ore which is typical primary niobium ore, wherein a large amount of carbonates such as calcite, dolomite and the like exist, the ore is basically not influenced by weathering, the oxidation degree is extremely low, and compared with the weathered niobium ore, the mineral composition and the properties have obvious difference, so that the process described in the text is not suitable for the beneficiation of the weathered niobium ore. There is no description at all of the recovery of weathered niobium ore.
CN103993162A discloses a method for removing iron and phosphorus from high-phosphorus ferroniobium concentrate, which adopts selective reduction and melting separation to realize the separation of iron phosphorus and niobium, and obtains phosphorus-containing pig iron and low-phosphorus and low-iron niobium slag. On the one hand, the processed objects are niobium-containing iron ore concentrate, but not weathered niobium ore mainly comprising pyrochlore, the obtained products are phosphorus-containing pig iron and low-phosphorus and low-iron niobium slag, but not corresponding niobium ore concentrate, iron ore concentrate and phosphorus ore concentrate, and more importantly, the adopted technology is pyrometallurgy at high temperature, but not physical ore dressing in the field of mineral processing.
Disclosure of Invention
The invention aims to solve the technical problem that a reasonable process technology is not available for treating weathered niobium ores mainly containing pyrochlore, so that niobium concentrate, iron concentrate and phosphorus concentrate cannot be obtained from the weathered niobium ores. Provides a beneficiation method of weathered niobium ores, and realizes effective recovery of niobium, iron and phosphorus in the weathered niobium ores.
The above purpose of the invention is realized by the following technical scheme:
a mineral processing method of weathered niobium ores comprises the following steps:
s1, grinding raw ore to-0.074 mm, wherein the ore accounts for 60-85%;
s2, adding water into the ground product, mixing the slurry until the concentration of the slurry is 15% -25%, and performing gravity separation to obtain gravity tailings and gravity coarse concentrate;
s3, carrying out magnetic separation on the gravity-separated rough concentrate obtained in the step S2 in a low-intensity magnetic separator, and adjusting the magnetic field intensity to be 0.15T-0.45T to obtain iron concentrate and low-intensity magnetic tailings;
s4, concentrating the weak magnetic tailings of the S3 to the concentration of 20-30% of ore pulp, adding 1000-3000 g/t of regulator according to the weight of ore feeding, stirring for 2-3 minutes, 200-500 g/t of collecting agent, stirring for 1-2 minutes, and performing rough concentration;
adding 100 g/t-200 g/t of collecting agent for primary scavenging;
adding collecting agent 60-120 g/t for secondary scavenging;
adding 400-800 g/t of regulator, and carrying out concentration for two to three times to obtain phosphate concentrate and phosphorus float tailings;
s5, concentrating and dewatering the float phosphorus tailings in the S4 until the concentration of ore pulp is 25% -35%, adding 2000-4000 g/t of regulator according to the weight of ore feeding, stirring for 2-3 minutes, stirring 200-600 g/t of collecting agent for 2-4 minutes, and performing rough concentration;
adding 100 g/t-200 g/t of collecting agent for primary scavenging;
adding 50-100 g/t of collecting agent for secondary scavenging;
adding 300 g/t-800 g/t of regulator, and carrying out concentration for three to four times to obtain niobium flotation concentrate and niobium flotation tailings.
The weathered niobium ore has the greatest characteristics of serious efflorescence, common argillization of gangue minerals, existence of a large amount of fine mud, and loss of selective separation effect of flotation due to the fact that the fine mud adsorbs medicaments and is not selectively covered on the surfaces of minerals. For gravity separation and magnetic separation, the existence of a large amount of fine mud causes the viscosity of ore pulp to increase, and the separation effect is also influenced due to serious inclusion among minerals. Therefore, the effective recovery of niobium from weathered niobium ores places high demands on the combination of beneficiation processes and beneficiation reagents.
The invention provides a beneficiation method for weathered niobium ore raw materials mainly comprising pyrochlore, which combines the special properties of weathered niobium ores and adopts a process of combining gravity separation, magnetic separation and flotation, so that ferrocolumbium and phosphorus in the ores are effectively recovered.
Wherein, the ore grinding in S1 has the following functions: the raw ore is ground to a suitable mineral grade, which may be, for example, 60%, 65%, 75% or 85% by-0.074 mm. The grinding treatment can obtain a proper ore dressing fraction, the grinding particle size is too fine, valuable minerals such as pyrochlore and the like are easily over-ground into a fine fraction, and then the fine fraction is lost and difficult to recover, so that the recovery rate is influenced, the grinding particle size is too coarse, the valuable minerals such as pyrochlore and the like are not dissociated, the high-grade niobium concentrate is difficult to obtain, and the recovery rate is influenced.
The role of reselection in S2 is: according to the specific gravity of valuable minerals such as pyrochlore, apatite and magnetite (hematite) which is greater than the specific gravity of gangue minerals such as clay and quartz, and the characteristic of light specific gravity of fine-particle argillaceous minerals, separation of the valuable minerals and the gangue minerals can be realized by gravity separation, and desliming is synchronously carried out to obtain gravity-separated rough concentrate.
And in the S2, the gravity concentration of the ore pulp is controlled to be 15% -25%, so that the gravity tailing/desliming can be better carried out.
The magnetic separation in S3 has the following functions: according to the fact that the magnetite (hematite) has strong magnetism, while the pyrochlore and the apatite generally have no magnetism or weak magnetism, the separation of the magnetite (hematite) from the pyrochlore and the apatite can be achieved by adopting magnetic separation, and meanwhile, an iron ore concentrate product is obtained, and comprehensive recovery of iron is achieved.
The magnetic field strength in S3 is more favorable for recovering magnetite (hematite).
The rough selection in S4 and S5 has the following functions:
the roughing in S4 is used for primarily realizing the enrichment of apatite to obtain the rough phosphorite flotation concentrate;
the rough concentration in S5 is used for primarily realizing the enrichment of pyrochlore and obtaining niobium flotation rough concentrate;
the effect of once scavenging is as follows: carrying out primary scavenging on valuable minerals which cannot be effectively recovered in roughing to enhance recovery so as to obtain primary scavenging concentrate;
the secondary scavenging has the following functions: carrying out secondary scavenging on valuable minerals which cannot be effectively recovered by primary scavenging to enhance recovery to obtain secondary scavenging concentrate;
the selection has the following functions: the grade of rough concentrate obtained by rough concentration usually cannot meet the quality requirement of the concentrate, and the final concentrate product can be obtained only by enhancing the separation between valuable minerals and gangue minerals and improving the grade through the concentration operation. According to the different requirements of the quality of the concentrate and the difficulty degree of the mineral separation, the times of the concentration operation are different, the higher the requirement of the quality of the concentrate is, the more difficult the mineral separation is, and the more the concentration times are needed.
The concentration of the ore pulp in the S4 is more favorable for floating phosphorus, and the concentration of the ore pulp in the S5 is more favorable for floating niobium.
Among other things, the gravity separation device of the present invention may be a spiral chute and/or a shaker.
Preferably, the original ore is ground to-0.074 mm in S1 to 85%, and the magnetic field intensity of the magnetic separation in S3 is 0.15T.
Preferably, the weathered niobium ore is Nb2O5The grade is 0.65-0.81%, the Fe grade is 18.93-26.17%, and P2O5The grade is 9.10-11.74%.
Preferably, the modifier in S4 is one or more of sodium carbonate, water glass and sodium hydroxide, and the collector is one or more of oleic acid, oxidized paraffin soap and tall soap.
Preferably, the coarse adjusting agent in S4 is a mixture of sodium carbonate or sodium hydroxide and water glass, and the ratio of sodium carbonate or sodium hydroxide: the mass ratio of the water glass is 1:3, and the collecting agent is oleic acid or a mixture of oxidized paraffin soap and tall soap, wherein the mass ratio of the oxidized paraffin soap: the mass ratio of the tall soap is 1: 1.
Preferably, the collector for the first scavenging and the second scavenging in S4 is oleic acid or a mixture of oxidized paraffin soap and tall soap, wherein the ratio of oxidized paraffin soap: the mass ratio of the tall soap is 1: 1.
Preferably, the selected modifier in S4 is a mixture of sodium carbonate and water glass or water glass, wherein the ratio of sodium carbonate: the mass ratio of the water glass is 1: 3-4.
Preferably, the modifier in S5 is one or more of hydrochloric acid, fluosilicic acid, tannic acid and sodium humate, and the collector is one or more of dodecylamine, octadecylamine, cocoamine and mixed amine.
Preferably, the roughing regulator in S5 is a mixture of hydrochloric acid and tannic acid or a mixture of fluosilicic acid and sodium humate, wherein the ratio of hydrochloric acid: the mass ratio of the tannic acid is 10:1, and the mass ratio of the fluosilicic acid: the mass ratio of the sodium humate is 80: 3; the collector is a mixture of dodecylamine and octadecylamine or a mixture of cocoamine and mixed amines, wherein the ratio of dodecylamine: the mass ratio of octadecylamine to cocoamine is 1: the mass ratio of the mixed amine is 1: 1.
Preferably, the collector for the first and second sweeps in S5 is a mixture of dodecylamine and octadecylamine or a mixture of cocoamine and mixed amines, wherein the ratio of dodecylamine: the mass ratio of octadecylamine to cocoamine is 1: the mass ratio of the mixed amine is 1: 1.
Preferably, the concentration modifier in S5 is a mixture of hydrochloric acid and tannic acid or a mixture of fluorosilicic acid and sodium humate, wherein the ratio of hydrochloric acid: the mass ratio of the tannic acid is 10-30: 1, and the mass ratio of the fluosilicic acid: the mass ratio of humic acid is 13-25: 1.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a beneficiation method of weathered niobium ores, which combines the special properties of weathered niobium ores and adopts a process of combining gravity separation, magnetic separation and flotation, so that the separation and recovery effect of niobium, iron and phosphorus is improved, wherein the grade of niobium concentrate is 46.35-51.27%, and Nb is Nb2O5The recovery rate is 58.12% -63.88%; the grade of the phosphate concentrate is 38.59-39.67%, P2O5The recovery rate is 68.68% -70.90%; the grade of the iron ore concentrate is 60.24-61.28%, the recovery rate of Fe is 53.54-57.68%, the difficult problem of separating and recovering gangue minerals, magnetite, apatite and pyrochlore in weathered niobium ores is effectively solved, iron and phosphorus are effectively recovered while niobium recovery is realized, and comprehensive recovery and utilization of mineral resources are realized.
Drawings
Fig. 1 is a schematic flow diagram of a beneficiation process of weathered niobium ore.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the present invention is not limited to the examples in any way. The starting reagents employed in the examples of the present invention are, unless otherwise specified, those that are conventionally purchased.
Example 1
A weathered niobium ore beneficiation method is shown in a flow chart of fig. 1, and comprises the following steps:
s1, grinding raw ore to-0.074 mm, wherein the raw ore accounts for 60%;
s2, adding water into the ground product, mixing the slurry until the concentration of the slurry is 15%, feeding the slurry into a spiral chute, and sorting to obtain gravity rough concentrate and gravity tailings;
s3, reselecting the rough concentrate and feeding the rough concentrate into a low-intensity magnetic separator for low-intensity magnetic separation, and adjusting the magnetic field intensity to be 0.15T to obtain iron concentrate and low-intensity magnetic tailings;
s4, concentrating the weak magnetic tailings until the concentration of the ore pulp is 20%, adding a floating phosphorus agent, and performing apatite flotation to obtain phosphorus concentrate and floating phosphorus tailings;
s5, concentrating the float phosphorus tailings to the pulp concentration of 25%, and adding a float niobium agent to obtain float niobium concentrate and float niobium tailings.
The specific medicament use cases are shown in table 1. The feeding ore is weathered niobium ore in Africa, and the specific properties are shown in Table 2.
Example 2
A mineral processing method of weathered niobium ores comprises the following steps:
s1, grinding raw ore to-0.074 mm, wherein the raw ore accounts for 85%;
s2, adding water into the ground product, mixing the slurry until the concentration of the slurry is 25%, feeding the slurry into a spiral chute, and sorting to obtain spiral rough concentrate and spiral tailings; feeding the spiral rough concentrate into a shaking table for sorting to obtain gravity rough concentrate and gravity tailings;
s3, reselecting the rough concentrate and feeding the rough concentrate into a low-intensity magnetic separator for low-intensity magnetic separation, and adjusting the magnetic field intensity to be 0.45T to obtain iron concentrate and low-intensity magnetic tailings;
s4, concentrating the weak magnetic tailings until the concentration of the ore pulp is 30%, adding a floating phosphorus agent, and performing apatite flotation to obtain phosphorus concentrate and floating phosphorus tailings;
s5, concentrating the float phosphorus tailings to the pulp concentration of 35%, and adding a float niobium agent to obtain float niobium concentrate and float niobium tailings.
The specific medicament use cases are shown in table 1. The feeding ore is weathered niobium ore in Africa, and the specific properties are shown in Table 2.
TABLE 1 dosage of the agents (g/ton. mineral feed)
TABLE 2
As can be seen from the above examples, the recovery method of the invention can well recover pyrochlore from weathered niobium ores, the obtained niobium concentrate has high grade, and Nb is2O5The grade can reach 51.27%, and the recovery rate reaches 63.38%. Meanwhile, the phosphorus and the iron in the ore are effectively recovered.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The ore dressing method for weathered niobium ore is characterized by comprising the following steps:
s1, grinding raw ore to-0.074 mm, wherein the ore accounts for 60-85%;
s2, adding water into the ground product, mixing the slurry until the concentration of the slurry is 15% -25%, and performing gravity separation to obtain gravity tailings and gravity coarse concentrate;
s3, carrying out magnetic separation on the gravity-separated rough concentrate obtained in the step S2 in a low-intensity magnetic separator, and adjusting the magnetic field intensity to be 0.15T-0.45T to obtain iron concentrate and low-intensity magnetic tailings;
s4, concentrating the weak magnetic tailings of the S3 to the concentration of 20-30% of ore pulp, adding 1000-3000 g/t of regulator according to the weight of ore feeding, stirring for 2-3 minutes, 200-500 g/t of collecting agent, stirring for 1-2 minutes, and performing rough concentration;
adding 100 g/t-200 g/t of collecting agent for primary scavenging;
adding collecting agent 60-120 g/t for secondary scavenging;
adding 400-800 g/t of regulator, and carrying out concentration for two to three times to obtain phosphate concentrate and phosphorus float tailings;
s5, concentrating and dewatering the float phosphorus tailings in the S4 until the concentration of ore pulp is 25% -35%, adding 2000-4000 g/t of regulator according to the weight of ore feeding, stirring for 2-3 minutes, stirring 200-600 g/t of collecting agent for 2-4 minutes, and performing rough concentration;
adding 100 g/t-200 g/t of collecting agent for primary scavenging;
adding 50-100 g/t of collecting agent for secondary scavenging;
adding 300 g/t-800 g/t of regulator, and carrying out concentration for three to four times to obtain niobium flotation concentrate and niobium flotation tailings.
2. The beneficiation method for weathered niobium ore according to claim 1, wherein the original ore is ground to 85% of-0.074 mm in S1, and the magnetic field intensity for magnetic separation in S3 is 0.15T.
3. The method for beneficiating weathered niobium ores as claimed in claim 1 wherein the weathered niobium ores are Nb2O5The grade is 0.65-0.81%, the Fe grade is 18.93-26.17%, and P2O5The grade is 9.10-11.74%.
4. The method for beneficiating weathered niobium ore as claimed in any one of claims 1 to 3, wherein said modifier is one or more of sodium carbonate, water glass and sodium hydroxide in S4, and said collector is one or more of oleic acid, oxidized paraffin soap and tall soap.
5. The method for beneficiating weathered niobium ore as claimed in claim 4, wherein said rougher conditioning agent in S4 is sodium carbonate or a mixture of sodium hydroxide and water glass, sodium carbonate or sodium hydroxide: the mass ratio of the water glass is 1:3, and the collecting agent is oleic acid or a mixture of oxidized paraffin soap and tall soap, wherein the mass ratio of the oxidized paraffin soap: the mass ratio of the tall soap is 1: 1.
6. The method for beneficiating weathered niobium ores as claimed in claim 5, wherein the collector for the first and second sweepings in S4 is oleic acid or a mixture of oxidized paraffin soap and tall soap, wherein the ratio of oxidized paraffin soap: the mass ratio of the tall soap is 1: 1.
7. The method for beneficiating weathered niobium ores as claimed in claim 6 wherein said beneficiating modifier in S4 is a mixture of sodium carbonate and water glass or water glass, wherein the ratio of sodium carbonate: the mass ratio of the water glass is 1: 3-4.
8. The method for beneficiating weathered niobium ore as claimed in any one of claims 1 to 3, wherein the conditioning agent in S5 is one or more of hydrochloric acid, fluosilicic acid, tannic acid and sodium humate, and the collecting agent is one or more of laurylamine, octadecylamine, cocoamine and mixed amine.
9. The method for beneficiating weathered niobium ores as claimed in claim 4, wherein said rougher conditioning agent in S5 is a mixture of hydrochloric acid and tannic acid or a mixture of fluorosilicic acid and sodium humate, wherein the ratio of hydrochloric acid: the mass ratio of the tannic acid is 10:1, and the mass ratio of the fluosilicic acid: the mass ratio of the sodium humate is 80: 3; the collector is a mixture of dodecylamine and octadecylamine or a mixture of cocoamine and mixed amines, wherein the ratio of dodecylamine: the mass ratio of octadecylamine to cocoamine is 1: the mass ratio of the mixed amine is 1: 1.
10. The method for beneficiating weathered niobium ores as claimed in claim 9, wherein the collectors of the primary and secondary scavenging in S5 are a mixture of dodecylamine and octadecylamine or a mixture of cocoylamine and mixed amines, wherein the ratio of dodecylamine: the mass ratio of octadecylamine to cocoamine is 1: the mass ratio of the mixed amine is 1: 1.
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| CN113304874A (en) * | 2021-04-29 | 2021-08-27 | 中国恩菲工程技术有限公司 | Flotation pretreatment method for niobium ores |
| WO2024164587A1 (en) * | 2023-02-09 | 2024-08-15 | 广东省科学院资源利用与稀土开发研究所 | Beneficiation method for recovering pyrochlore from high-silicon high-calcium carbonatite-type niobium ore |
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