CN109266841B - Roasting treatment method of iron tailings - Google Patents
Roasting treatment method of iron tailings Download PDFInfo
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- CN109266841B CN109266841B CN201811427866.5A CN201811427866A CN109266841B CN 109266841 B CN109266841 B CN 109266841B CN 201811427866 A CN201811427866 A CN 201811427866A CN 109266841 B CN109266841 B CN 109266841B
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- roasting
- iron tailings
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- chlorinating agent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
- C22B1/08—Chloridising roasting
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a roasting treatment method of iron tailings, which comprises the following steps: the method comprises the following steps: roasting: roasting the iron tailings in an inert gas atmosphere, and carrying out temperature programmed heating and temperature programmed cooling; and (3) recovering: and recovering the volatilized flue gas to obtain metal chloride, taking out the roasting slag after the roasting temperature in the S1 is reduced to 50-150 ℃, and carrying out magnetic separation on the roasting slag to obtain magnetite. According to the invention, through specific inert gas roasting atmosphere, the addition amount of a chlorinating agent and roasting temperature rise and fall program control, the magnetization separation of the iron tailings is realized, good iron ore magnetization and valuable metal separation effects are achieved, the removal rates of lead, copper, zinc and cadmium respectively reach 98.89%, 66.71%, 60.51% and 96.6%, the magnetic separation recovery rate reaches 98.29%, a reducing agent is not required to be added, the magnetization of iron in the tailings is realized by controlling the roasting atmosphere, the problems of large pollution in the iron tailings treatment process and influence on the recovery of metal in flue gas are fundamentally reduced, the operation is simple and convenient, the cost is lower, and the reduction and recycling benefits of the iron tailings are obvious.
Description
Technical Field
The invention belongs to the field of comprehensive utilization of tailing resources, and particularly relates to a roasting treatment method of iron tailings.
Background
China is the second largest iron ore producing country in the world next to Brazil, and iron tailings contain a large amount of elements such as Fe, Cu, Zn, S and the like, so that the large amount of stored iron tailings not only causes great resource waste, but also causes great threat and harm to the environment. Environmental responsibility and sustainable development of mineral resources are of great importance to the mining industry, so how to safely dispose and utilize iron tailings as resources is a challenging task faced by China. For a long time, the iron tailings are treated by stacking and burying, which not only occupies a large space, but also increases the treatment cost and has potential threat to the environment.
Patent CN101225468 discloses a method for recovering gold, silver, iron and lead from acidified roasting slag by a magnetization chlorination process, and patent CN105671305A discloses a method for preparing ferronickel fine powder by roasting and reducing laterite-nickel ore by using chlorine salt. However, carbon reducing agents such as carbon powder and the like are required to be added in the treatment process, the operation is complex, the additive cost is high, the roasting energy consumption is high, the carbon content in the flue gas is high, the pollution in the process is great, and the recovery of metals in the flue gas is influenced.
Therefore, it is important to provide a method for treating the iron tailings with less pollution without adding a carbonaceous reducing agent.
Disclosure of Invention
The invention provides a roasting treatment method of iron tailings to overcome the defects in the prior art. The method has simple process, does not need to add a reducing agent, avoids the problems of large smoke pollution, low metal recovery rate and the like, and synchronously carries out chlorination roasting and volatilization treatment on copper, lead, zinc and cadmium elements in the iron tailings and iron in the magnetized iron tailings.
The above purpose of the invention is realized by the following technical scheme:
a method for treating iron tailings comprises the following steps:
s1, roasting: mixing the iron tailings with a chlorinating agent, and then roasting in an inert gas atmosphere, wherein the gas flow rate is 20-200 ml/min, and the roasting conditions are as follows: heating and cooling by a program, wherein the heating rate is 2-10 ℃/min, the heat preservation is 30-120 min, the cooling rate is 3-10 ℃/min, and the roasting temperature is 500-1200 ℃;
s2, recovery: and recovering the volatile flue gas to obtain chlorides of copper, lead, zinc and cadmium, and after the roasting temperature in the S1 is reduced to 50-150 ℃, taking out the roasted slag, grinding the slag, and performing magnetic separation to obtain magnetite.
Compared with the existing chlorination and magnetization roasting technology, the chlorination and magnetization roasting technology of the invention does not need to add a reducing agent, avoids pollution and energy consumption caused by adding reducing agents such as carbon powder and the like, realizes good magnetization of iron by controlling roasting atmosphere and roasting temperature rise and drop programs, and further obtains other metal chlorides and magnetized iron ore by subsequent volatile smoke recovery and magnetic separation. In the chloridizing roasting process, the chloridizing agent is added, and the chloridizing agent and lead, cadmium, copper and zinc in the tailings are converted into corresponding metal chlorides at high temperature, and the corresponding metal chlorides are volatilized out by virtue of the low boiling point characteristic of the corresponding metal chlorides; meanwhile, under the inert atmosphere, the oxidation reaction in the roasting process is inhibited, the conversion of iron elements in the iron tailings is promoted, and the goethite and the pyrite in the tailings are converted into magnetite through a certain reaction.
According to the roasting treatment, a chlorinating agent and iron tailings are uniformly mixed, a specific roasting program is set, the roasting volatilization is carried out under the inert gas atmosphere at a certain temperature rising rate, heat preservation time and temperature lowering rate, volatile components and roasting slag are obtained, wherein the roasting atmosphere, the adding amount of the chlorinating agent and the specific roasting temperature rising and falling process setting are all important parameters influencing the magnetizing roasting of the iron tailings, the specific roasting effect of the invention is realized through the comprehensive action of the important parameters, and the efficient recovery of magnetite and valuable metals is realized. The roasting slag is magnetized in the roasting process, and the magnetized Fe in the roasting slag3O4Can be further separated by magnetic separation. The method has the advantages that the reducing agent is not needed to be added in the chlorination roasting process, and the iron tailings are ferromagnetized by controlling the chlorination roasting atmosphere, so that harmlessness, reduction to a greater extent and recycling of the iron tailings are realized.
The inert gas is preferably nitrogen, and the iron tailings are ground and sieved by a 100-mesh sieve.
Preferably, the gas flow rate in S1 is 20-100 mL/min.
Preferably, the roasting temperature in S1 is 600-1000 ℃. For example, 600 ℃, 700 ℃, 800 ℃, 900 ℃ or 1000 ℃ may be used. When the roasting temperature is lower, the chlorination effect is poorer, the chlorination volatilization of metals such as copper, lead, zinc and the like is not facilitated, the very high chlorination volatilization effect is achieved at 1000 ℃, when the temperature is too high, the cost is improved, but the space for improving the chlorination magnetization effect is lower.
More preferably, the firing temperature in S1 is 1000 ℃.
More preferably, the temperature programming in S1 includes the steps of: heating to 600-700 ℃ at a rate of 5-8 (5 ℃/min), heating to 700-850 (800 ℃) at a rate of 3-5 (3 ℃/min), and heating to 850-1000 ℃ at a rate of 2-3 (2 ℃/min).
The temperature is raised in stages to protect the tubular electric furnace, and the temperature raising speed is preferably: the temperature is raised to 600-700 ℃ at the rate of 5 ℃/min, then to 800 ℃ at the rate of 3 ℃/min, and finally to 850-1000 ℃ at the rate of 2 ℃/min.
Preferably, the iron tailings in the S1 are firstly mixed with a chlorinating agent and then roasted, and the addition amount of the chlorinating agent is 0.1-20%. For example, the concentration may be 5%, 7.5%, 10%, 15%, and the chlorinating agent is a chloride salt, preferably anhydrous calcium chloride.
The chlorinating agent is added to promote the chlorination volatilization of metals such as lead, cadmium, copper, zinc and the like in the iron tailings and has certain influence on the magnetization of iron in the iron tailings. When the chlorinating agent is added too much, the cost is high, the chlorination volatilization effect is not obviously improved, more calcium elements are remained in the roasting slag, and the magnetization separation effect of the roasting slag is reduced.
More preferably, the amount of the chlorinating agent added in S1 is 0.1% to 7.5%. The inventors have discovered unexpectedly that when the amount of the chlorinating agent is 7.5% or less, the magnetization effect is better and the magnetic separation recovery rate is higher.
More preferably, the chlorinating agent is added in an amount of 5% in S1. When the addition amount of the chlorinating agent is 5%, the roasted residue is subjected to magnetic separation, and the magnetic separation recovery rate is highest and can reach 98.29%.
Preferably, the mixing of the iron tailings and the chlorinating agent in the S1 is wet mixing, and comprises the following steps: and adding water into the chlorinating agent for complete dissolution, adding the iron tailings for uniform mixing, and drying to obtain a sample to be roasted. The wet mixing is beneficial to more uniform mixing of the iron tailings and the chlorinating agent.
More preferably, the solid-liquid ratio of the total mass of the chlorinating agent and the iron tailings to water is 1: 3-3: 1 g/mL.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method for treating iron tailings by specific treatmentThe inert gas roasting atmosphere and the specific roasting temperature rise program control realize the magnetization separation of the iron tailings, and achieve good iron ore magnetization and valuable metal separation effects, by adopting the treatment method, the removal rates of lead, copper, zinc and cadmium respectively reach 98.89%, 66.71%, 60.51% and 99.61%, and the roasting slag obtained by recovery mainly comprises Fe3O4And SiO2And (4) forming. The recovery method provided by the invention does not need to add a reducing agent, realizes the magnetization of iron in the tailings by controlling the roasting atmosphere, fundamentally avoids the problems of large pollution in the iron tailing treatment process and influence on the recovery of metals in the flue gas, is simple and convenient to operate, has low cost, and has obvious reduction and recycling benefits on the iron tailings.
Drawings
Fig. 1 is a process flow diagram of the treatment method of the iron tailings.
FIG. 2 is a diagram showing the result of XRD test of iron tailings of a certain mine.
FIG. 3 is a chart showing the results of XRD measurement of the roasting slag obtained in examples 1 to 3.
Detailed Description
In order to more clearly and completely describe the technical scheme of the invention, the invention is further described in detail by the specific embodiments, and it should be understood that the specific embodiments described herein are only used for explaining the invention, and are not used for limiting the invention, and various changes can be made within the scope defined by the claims of the invention. The source of the preparation raw material of the present invention is not particularly limited, and may be commercially available.
The iron tailing raw material is taken from a certain mine, and the XRD test result graph of the iron tailing is shown in figure 2.
Example 1
A roasting treatment method of iron tailings, wherein a recovery process flow is shown in figure 1, and comprises the following steps:
s1, roasting: mixing 8.5g of iron tailings and 1.5g of chlorinating agent, adding 13ml of ultrapure water, drying at 105 ℃ for 15h, and roasting in an inert gas atmosphere, wherein the gas flow rate is 50ml/min, and the roasting conditions are as follows: heating to 600 ℃ at the speed of 5 ℃/min, heating to 800 ℃ at the speed of 3 ℃/min, heating to 1000 ℃ at the speed of 2 ℃/min, cooling at the speed of 5 ℃/min, roasting at the temperature of 1000 ℃, and keeping the temperature for 60 min;
s2, recovery: and (4) after the roasting temperature in the S1 is reduced to 120 ℃, condensing the volatilized flue gas, collecting partial copper, lead, zinc and cadmium elements, and carrying out magnetic separation on the roasting slag to obtain magnetite.
Example 2
A roasting treatment method of iron tailings comprises the following steps:
s1, roasting: mixing 17g of iron tailings and 3g of chlorinating agent, adding 25ml of ultrapure water, drying at 105 ℃ for 35 hours, and roasting in an inert gas atmosphere, wherein the gas flow rate is 100ml/min, and the roasting conditions are as follows: heating to 600 ℃ at the speed of 5 ℃/min, heating to 800 ℃ at the speed of 3 ℃/min, cooling at the speed of 5 ℃/min, roasting at the temperature of 800 ℃, and keeping the temperature for 60 min;
s2, recovery: and (4) after the roasting temperature in the S1 is reduced to 120 ℃, condensing the volatilized flue gas to obtain partial copper, lead, zinc and cadmium elements, and carrying out magnetic separation on the roasting slag to obtain magnetite.
Example 3
A roasting treatment method of iron tailings comprises the following steps:
s1, roasting: mixing 17g of iron tailings and 3g of chlorinating agent, adding 25ml of ultrapure water, drying at 105 ℃ for 35 hours, and roasting in an inert gas atmosphere, wherein the gas flow rate is 100ml/min, and the roasting conditions are as follows: adopting program heating and program cooling, wherein the heating rate is 5 ℃/min, the cooling rate is 5 ℃/min, the roasting temperature is 600 ℃, and the heat preservation time is 60 min;
s2, recovery: and (4) after the roasting temperature in the S1 is reduced to 120 ℃, condensing the volatilized flue gas to obtain partial copper, lead, zinc and cadmium elements, and carrying out magnetic separation on the roasting slag to obtain magnetite.
Examples 4 to 8
A roasting treatment method of iron tailings is basically the same as that of example 1, and the differences are shown in Table 1.
TABLE 1
| Item | Amount of chlorinating agent added (%) | Gas flow rate (ml/min) | Calcination temperature (. degree.C.) |
| Example 4 | 5 | 50 | 1000 |
| Example 5 | 7.5 | 50 | 1000 |
| Example 6 | 10 | 50 | 1000 |
| Example 7 | 5 | 40 | 800 |
| Example 8 | 5 | 60 | 600 |
Comparative example 1
The roasting treatment method of the iron tailings is characterized by comprising the following steps:
s1, roasting: adding a carbon powder reducing agent into the iron tailings for roasting, wherein the roasting temperature is 1000 ℃;
s2, recovery: and recovering the volatile flue gas to obtain chlorides of copper, lead, zinc and cadmium, and after the roasting temperature in the S1 is reduced to 50-150 ℃, taking out the roasted slag, grinding the slag, and performing magnetic separation to obtain magnetite.
Result detection
XRD (X-ray diffraction) tests were carried out on the roasting slag obtained in examples 1 to 3, and the test results are shown in FIG. 3.
As shown in FIG. 3, the main component of the roasted slag is Fe3O4And SiO2And with increasing temperature, Fe3O4The responsivity of the diffraction peak is stronger and stronger, which shows that the temperature has a positive influence on the chloridizing magnetization of the iron tailings in a certain temperature range.
The removal rate of lead, copper, zinc and cadmium and the magnetic separation recovery rate of the roasting slag in the examples and the comparative examples are calculated, and the calculation formula is as follows:
(1)
wherein: c, the concentration (mg/Kg) of metal in the iron tailings; m is the addition amount (g) of the iron tailings; c, the metal concentration (mg/Kg) in the residue after roasting; m is the mass (g) of the residue after calcination.
(2) Magnetic separation recovery rate is m0/m 1100% of, wherein m0: mass (g) of magnetic separator; m is1Weighing the mass (g) of the residue after roasting.
The results of the removal rate of lead, copper, zinc and cadmium and the magnetic separation recovery rate are shown in Table 3.
TABLE 3
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. It will be understood by those skilled in the art that various other changes and modifications may be made in the above-described embodiments, and it is not necessary, nor is it intended to be 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 roasting treatment method of the iron tailings is characterized by comprising the following steps:
s1, roasting: mixing the iron tailings with a chlorinating agent, and then roasting in an inert gas atmosphere, wherein the gas flow rate is 20-200 ml/min, and the roasting conditions are as follows: heating and cooling by a program, wherein the heating rate is 2-10 ℃/min, the heat preservation is 30-120 min, the cooling rate is 3-10 ℃/min, and the roasting temperature is 500-1200 ℃;
s2, recovery: and (3) recovering chlorides of copper, lead, zinc and cadmium in the volatile flue gas, taking out the roasting slag after the roasting temperature in S1 is reduced to 50-150 ℃, and carrying out magnetic separation after grinding to obtain magnetite.
2. The roasting treatment method according to claim 1, wherein the gas flow rate in S1 is 20 to 100 mL/min.
3. The roasting treatment method according to claim 1, wherein the roasting temperature in S1 is 600 to 1000 ℃.
4. The firing treatment method as recited in claim 3, wherein the temperature programming at S1 includes the steps of: heating to 500-700 ℃ at a speed of 5-8 ℃/min, heating to 700-850 ℃ at a speed of 3-5 ℃, and finally heating to 850-1200 ℃ at a speed of 2-3 ℃.
5. The roasting treatment method according to claim 1, wherein the chlorinating agent is added in an amount of 0.1% to 20% in S1.
6. The roasting treatment method according to claim 5, wherein the chlorinating agent is added in an amount of 0.1% to 7.5% in S1.
7. The roasting treatment method according to claim 6, wherein the chlorinating agent is added in an amount of 5% in S1.
8. The roasting treatment method of claim 5, wherein the mixing of the iron tailings and the chlorinating agent in the S1 is wet mixing, and the method comprises the following steps: and adding water into the chlorinating agent for complete dissolution, adding the iron tailings for uniform mixing, and drying to obtain a sample to be roasted.
9. The roasting treatment method according to claim 8, wherein the solid-to-liquid ratio of the total mass of the chlorinating agent and the iron tailings to water is 1: 3-3: 1 g/mL.
10. The roasting treatment method according to any one of claims 1 to 9, wherein the volatile flue gas is recovered in S2 as a condensation recovery and a wet absorption recovery.
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| CN111979422B (en) * | 2020-07-09 | 2022-10-21 | 有研资源环境技术研究院(北京)有限公司 | Method for comprehensively recovering valuable metals in goethite slag |
| CN113546952B (en) * | 2021-06-02 | 2022-07-01 | 华南师范大学 | Magnetic biochar soil remediation agent for soil heavy metal pollution and application thereof |
| CN114645133A (en) * | 2022-03-21 | 2022-06-21 | 冯垚 | Magnetizing roasting method for stockpiled tailings |
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| CN114941075B (en) * | 2022-05-30 | 2023-06-27 | 金川镍钴研究设计院有限责任公司 | Nickel slag impurity removal method |
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