CN113061715B - Sodium iron polysulfide additive for strengthening low-temperature rapid reduction of refractory iron ore and application method thereof - Google Patents
Sodium iron polysulfide additive for strengthening low-temperature rapid reduction of refractory iron ore and application method thereof Download PDFInfo
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Abstract
The invention relates to an additive for strengthening solid reduction of refractory iron ore and application thereof: the additive contains Na, Fe and S; the valence state of S in the additive is less than 0, and the Na, the Fe and the S exist in the form of compounds. The application method of the additive comprises the following steps: uniformly mixing fine-fraction refractory iron ore and a sodium iron polysulfide additive for agglomeration, drying the obtained agglomerate, placing the dried agglomerate in a reducing atmosphere for high-temperature roasting, and grinding and magnetically separating the cooled roasted product to obtain a magnetic metal iron/iron alloy product and nonmagnetic tailings. The non-magnetic tailings containing sodium, iron and sulfur can be further separated to recover sodium iron polysulfide, so that the additive can be recycled. The additive is mainly obtained from metallurgical solid waste, is low in price and environment-friendly, can provide technical support for efficient utilization of iron ores which are difficult to treat, has the advantage of synergistic treatment of the solid waste, is easy to realize industrialization, and has very wide popularization and application prospects.
Description
Technical Field
The invention relates to an additive for strengthening solid reduction of iron ore and application thereof, in particular to a sodium iron polysulfide additive for strengthening low-temperature rapid reduction of refractory iron ore and application thereof.
Background
The iron ore resource reserves in China are rich, but the iron ore has the characteristics of poor quality, fine quality, impurity and the like, and the economical recoverable reserves are less, and the lean ores are more and the rich ores are less; associated ores are numerous, the difficulty of selection and smelting is high, and the development and utilization cost is high. In recent years, the solid-state reduction roasting-sorting process is widely applied to the treatment of complex iron ore resources due to the advantages of simple process, short flow, low operation cost and the like. However, since the subsequent physical separation process has higher requirements on the size of the metallic iron grains, the aggregation and growth of the metallic iron grains must be realized in the reduction roasting process, otherwise, the problems of poor separation effect, low recovery rate of valuable metals, low product quality and the like are caused.
The means for strengthening the solid reduction of the iron ore difficult to treat mainly comprises the steps of improving the roasting temperature, prolonging the roasting time, adding proper additives and the like.
The energy consumption is increased by enhancing the reduction by increasing the roasting temperature, and the materials are easy to melt; the production efficiency is reduced and the energy consumption is increased by prolonging the roasting time; the addition of proper additives is considered to be the most effective method, and the research work is more, particularly, the additive containing sodium, sulfur and other components has the most obvious effect. For example, the sodium salt modified paigeite and the application thereof in the reduction and separation of the iron-containing resources difficult to treat (application number: 201210191947.6), the paigeite is mixed with sodium sulfate and sodium carbonate with certain mass ratio and agglomerated, and the dried agglomerate is reduced and roasted to prepare the sodium salt modified paigeite which can promote the aggregation and growth of metal iron grains in the reduction process of the iron-containing resources difficult to treat; an additive for strengthening the reduction and separation of laterite-nickel ore (application number: CN200810143854.X), which is prepared by uniformly mixing anhydrous sodium sulphate, soda, borax, sodium oxalate and sodium humate with laterite-nickel ore according to a certain mass ratio, agglomerating, reducing and roasting, wherein the used additive can promote the growth of nickel and iron grains in the reduction process, and realize the efficient separation of nickel, iron and impurities. Research results show that sodium sulfate is added into iron ore which is difficult to treat, Fe-FeS eutectic point compounds can be formed, and the reflow characteristic temperature of the system is remarkably reduced. Although the additive has a certain effect on strengthening the solid reduction of the iron ore which is difficult to treat, the production process of the used additive is complicated or the cost is high.
The reserve of high-sulfur bauxite which is proved to be more than 5.6 hundred million tons in China, and the direct treatment of the high-sulfur bauxite by the Bayer process can increase alkali consumption and corrode equipment, and desulfurization treatment is required. The sulfur in the sodium aluminate solution is removed by adopting an iron-based desulfurizer, and the desulfurization efficiency can reach 70-90%. The main component of the desulphurization slag is sodium iron polysulfide (NaFeS)2) Or hydrated sodium iron polysulphides (NaFeS)2·2H2O). Since the desulfurization slag causes environmental pollution if not disposed of properly, many researchers have studied a method for treating the desulfurization slag. For example, in the method for comprehensively treating the sulfur and the iron in the sodium aluminate solution based on the regenerable sulfur removal agent (application number: CN104591246A), the sulfur element in the desulfurized slag is oxidized into elemental sulfur by oxidizing the desulfurized slag, and the separation of the sulfur and the iron is realized by flotation, the method is carried out in an acid system, and the desulfurized slag enters the acid oxidation system from an alkaline system of a Bayer process and then returns to the alkaline systemIn addition, a large amount of acid and alkali are consumed, and the separation of sulfur and iron after flotation is not complete; "regeneration cycle of iron-based desulfurized slag" ("proceedings of Process engineering" 2017,17(6)) oxidizing desulfurized slag in alkaline system to make sulfur in desulfurized slag S2O3 2-The form of the iron-containing solid phase enters a liquid phase, and the iron-containing solid phase is converted into FeOOH in the regeneration process of the desulfurization slag and can be returned for circular desulfurization; the method comprises the steps of preparing sodium ferrite by regenerating iron-based desulfurization slag and performing cyclic desulfurization of the sodium ferrite (proceedings of Process engineering 2018,18(6)) removing most of sulfur in the desulfurization slag through oxidizing roasting, further deeply removing sulfur through water leaching, and regenerating the leaching slag to synthesize the sodium ferrite for the cyclic desulfurization. The method for treating the desulfurization slag needs to realize the oxidation of the desulfurization slag in an acid system, an alkaline system or high-temperature roasting and then carry out iron-sulfur separation, and has complex flow and higher production cost.
At present, more than 80 percent of lead resources worldwide come from the recovery of lead-acid batteries, and the pyrogenic process treatment is the most economic and effective treatment means. During the alkali fusion treatment, carbon is used as a reducing agent, iron is used as a sulfur-fixing agent, sodium carbonate is used as a fluxing agent, 300-350 kg of desulfurization solid waste is generated every ton of lead is produced, and the main component of the desulfurization solid waste is sodium iron polysulfide. The main reaction of the alkali fusion method is as follows:
2PbSO4+Na2CO3+Fe+9C＝2Pb+FeS·Na2S+9CO+CO2
the desulfurization slag has unstable property and certain toxicity, has great harm to the environment, and a plurality of researchers research the method for reducing the generation of the desulfurization slag or reducing the toxicity of the desulfurization slag in the alkali fusion process.
In addition, other non-ferrous metallurgy fields also produce similar desulphurisation slags containing sodium iron polysulphides. The metallurgical solid waste is difficult to treat, occupies land and pollutes the environment after being accumulated for a long time.
The invention is especially provided for solving the problems of poor solid reduction effect of iron ore and complex additive production process or higher cost which are difficult to treat, and simultaneously economically and reasonably disposing and utilizing metallurgy solid waste containing sodium iron polysulfide.
Disclosure of Invention
The invention aims to solve the first technical problem of providing a sodium iron polysulfide additive which has reasonable components, low price, simple production process, environmental protection and capability of effectively strengthening the low-temperature rapid reduction of iron ores difficult to treat.
The second technical problem to be solved by the invention is to provide an application method of the sodium iron polysulfide additive.
In order to solve the first technical problem, the sodium iron polysulfide additive for strengthening the low-temperature rapid reduction of the iron ore difficult to treat provided by the invention can be further separated and extracted from the solid reduction-magnetic separation tailings of the iron ore difficult to treat or directly use metallurgical solid waste containing sodium iron polysulfide, in particular desulfurization solid waste in the field of nonferrous metals.
In order to solve the second technical problem, the application of the sodium iron polysulfide additive for strengthening the low-temperature rapid reduction of the refractory iron ore provided by the invention comprises the steps of uniformly mixing fine-grained refractory iron ore and the sodium iron polysulfide additive for agglomeration, drying the obtained agglomerate, placing the dried agglomerate in a reducing atmosphere for high-temperature roasting, and grinding and magnetically separating the cooled roasted product to obtain a magnetic iron-containing product and nonmagnetic tailings. The nonmagnetic tailings can be further separated and extracted to generate sodium iron polysulfide from sodium, iron and sulfur components, so that the functional components of the additive can be recycled.
The invention relates to an additive for strengthening low-temperature rapid reduction of refractory iron ore, which contains Na, Fe and S; the occurrence valence of S in the additive is less than 0, and the Na, the Fe and the S exist in the form of compounds.
As one preferable scheme, the additive for strengthening the low-temperature rapid reduction of the refractory iron ore contains NaFeS2。
As one of the preferable schemes, the invention relates to an additive for strengthening the low-temperature rapid reduction of refractory iron ore, and the main component of the additive is sodium iron polysulfide (NaFeS)2) And/or hydrated sodium iron polysulphides (NaFeS)2·2H2O)。
As one of the preferable schemes, the additive for strengthening the low-temperature rapid reduction of the iron ore difficult to treat, namely the desulfurization slag generated in the process of producing alumina by the Bayer process of the high-sulfur bauxite, the desulfurization slag generated in the process of recovering the lead-acid battery by the alkali fusion method and the desulfurization slag containing sodium iron polysulfide generated in the smelting process of other nonferrous metals can be directly used as the additive.
The invention relates to an application method of an additive for strengthening low-temperature rapid reduction of refractory iron ores, which comprises the steps of mixing the refractory iron ores and the additive for agglomeration, drying the obtained agglomerates, roasting in a reducing atmosphere at the roasting temperature of 1000-1100 ℃ for 60-120 min, grinding and magnetically separating the cooled roasted products to obtain magnetic metal iron/iron alloy products and nonmagnetic tailings.
The invention relates to an application method of an additive for strengthening low-temperature rapid reduction of refractory iron ore.
The application method of the additive for strengthening the low-temperature rapid reduction of the iron ore difficult to treat comprises the following steps of grinding the iron ore difficult to treat to be less than 100 meshes in a fine mode, wherein the dosage of the additive is 5-30% of the mass ratio of the iron ore difficult to treat, preferably 8-20%.
The invention relates to an application method of an additive for strengthening the low-temperature rapid reduction of a refractory iron-containing resource, and after roasting, the average particle size of the obtained metallic iron particles is more than or equal to 45 mu m.
The invention relates to an application method of an additive for strengthening low-temperature rapid reduction of refractory iron ore, which is characterized in that after the additive is used for treating iron ore A, the recovery rate of iron is more than or equal to 91%, the iron ore A does not contain laterite nickel ore, and when the iron ore is laterite nickel ore, the recovery rate of Ni is more than or equal to 92%.
According to the application method of the additive for strengthening the low-temperature rapid reduction of the iron ore difficult to treat, when the iron ore contains boron, the dissolution rate of the boron is more than or equal to 92% after the iron ore is treated by the additive;
when the iron ore contains niobium, the removal rate of the Nb is more than or equal to 90 percent after the iron ore is treated by the additive;
when the iron ore contains phosphorus, the P removal rate is more than or equal to 90 percent after the iron ore is treated by the additive.
The sodium iron polysulfide additive for strengthening the low-temperature rapid reduction of the iron ore difficult to treat by adopting the technical scheme and the application thereof have the following technical principles in brief:
the main component of the additive is sodium iron polysulfide (NaFeS)2) Or hydrated sodium iron polysulphides (NaFeS)2·2H2O), the sodium component is used for strengthening the metallization reduction of metal oxides in the complex iron-containing minerals, the iron and sulfur components are used for forming Fe-FeS low-melting-point eutectic (melting point 985 ℃) micro-zone melt with the metal iron particles, better dynamic conditions are provided for the migration and growth of the iron/alloy particles, and the aggregation and growth of the metal iron/alloy particles are promoted.
NaFeS2·2H2O＝NaFeS2+2H2O
NaFeS2＝Na2S+FeS
FeO+Na2S＝FeS+Na2O
FeO·SiO2+Na2O＝Fe+Na2SiO3
FeO·Al2O3+Na2O＝Fe+2NaAlO2
MgO·B2O3+Na2O＝MgO+Na2O·B2O3
2Fe2O3+3C＝4Fe+3CO2
The invention has the advantages that:
1) the additive has reasonable components, low price and simple production process;
2) the additive can be directly used in the waste (NaFeS) generated in the prior art2And/or NaFeS2·2H2The metallurgical solid waste with O as the main component) realizes the ingenious conversion of changing waste into valuable.
3) The main constituent elements of the sodium iron polysulfide additive, namely sodium, sulfur and iron, are skillfully utilized to synergistically strengthen the metallization reduction of iron oxide in complex iron-containing minerals and promote the aggregation and growth of iron grains, and the strengthening effect is obvious;
4) the sodium iron polysulfide additive can be obtained by separating and extracting from the refractory iron ore solid reduction-ore grinding magnetic separation tailings or directly uses the metallurgical solid waste containing sodium iron polysulfide, and simultaneously plays roles in strengthening the refractory iron ore solid reduction and cooperatively treating the metallurgical solid waste, thereby being green and environment-friendly.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1:
TFe content of a high-alumina iron ore is 48.9%, Al2O3The content is 8.2 percent, the finely ground iron ore and 15 percent of sodium iron polysulfide additive are mixed uniformly for agglomeration, the obtained agglomerate is dried and then is reduced and roasted by adopting brown coal as a reducing agent, the roasting temperature is 1050 ℃, and the roasting time is 90 min. Compared with the method without adding the desulphurization slag, the average grain diameter of the metallic iron grains in the roasted ore is increased from 5 mu m to 46 mu m, and the subsequent iron and aluminum separation effect can be effectively improved. The iron grade of the magnetic concentrate is 91.2 percent and Al2O3The content is 1.30%, the iron recovery rate is 91.7%, and the aluminum removal rate is 91.0%.
Comparative example 1
The other conditions were the same as in example 1 except that the sodium iron polysulfide additive was used in an amount of 3%; the iron grade of the magnetic concentrate is 82.3 percent and Al2O3The content is 4.40%, the iron recovery rate is 81.5%, and the aluminum removal rate is 55.2%.
Comparative example 2
The other conditions were the same as in example 1 except that the sodium iron polysulfide additive was used in an amount of 35%. The iron grade of the magnetic concentrate is 92.2 percent and Al2O3The content is 1.2%, the iron recovery rate is 85.7%, and the aluminum removal rate is 92.6%.
Example 2:
the TFe content of a certain laterite-nickel ore is 22.1%, the Ni content is 1.91%, the finely ground laterite-nickel ore and 20% of sodium iron polysulfide additive are mixed uniformly for agglomeration, the obtained agglomerate is dried and then is reduced and roasted by adopting lignite as a reducing agent, the roasting temperature is 1100 ℃, and the roasting time is 60 min. Compared with the method without adding the desulphurization slag, the average grain diameter of the ferronickel alloy grains in the roasted ore is increased from 7 mu m to 52 mu m, and the subsequent separation effect of ferronickel and gangue components can be effectively improved. The iron grade of the magnetic concentrate is 80.0 percent, the nickel grade is 9.8 percent, the iron recovery rate is 56.9 percent, and the nickel recovery rate is 92 percent.
Comparative example 3
The other conditions were the same as in example 2 except that the sodium iron polysulfide additive was used in an amount of 3%; the iron grade of the magnetic concentrate is 68.1%, the nickel grade is 4.2%, the iron recovery rate is 55.3%, and the nickel recovery rate is 79.5%.
Comparative example 4
The other conditions were the same as in example 2 except that the sodium iron polysulfide additive was used in an amount of 35%; the iron grade of the magnetic concentrate is 88.9 percent, the nickel grade is 10.4 percent, the iron recovery rate is 48.2 percent, and the nickel recovery rate is 93.6 percent.
Example 3:
the method comprises the steps of enabling the TFe content of certain high-phosphorus oolitic hematite to be 49.0% and the P content to be 1.6%, evenly mixing ground high-phosphorus oolitic hematite with 8% of multi-sulfur iron sodium additive in mass ratio to form blocks, drying the obtained blocks, and then carrying out reduction roasting by using anthracite as a reducing agent, wherein the roasting temperature is 1050 ℃, and the roasting time is 120 min. Compared with the method without adding the desulphurization slag, the average grain diameter of the metallic iron grains in the roasted ore is increased from 9 mu m to 48 mu m, and the subsequent iron and phosphorus separation effect can be effectively improved. The iron grade of the magnetic concentrate is 92.7%, the phosphorus content is 0.09%, the iron recovery rate is 92.5%, and the phosphorus removal rate is 96.1%.
Comparative example 5
The other conditions were the same as in example 3 except that the sodium iron polysulfide additive was used in an amount of 3%; the iron grade of the magnetic concentrate is 83.7%, the phosphorus content is 0.69%, the iron recovery rate is 82.8%, and the phosphorus removal rate is 66.2%.
Comparative example 6
The other conditions were the same as in example 3 except that the sodium iron polysulfide additive was used in an amount of 35%; the iron grade of the magnetic concentrate is 88.6 percent, the phosphorus content is 0.35 percent, the iron recovery rate is 85.4 percent, and the phosphorus removal rate is 86.2 percent.
Example 4:
TFe content of a paigeite is 52.1%, B2O3The content of the active carbon is 5.3 percent,evenly mixing the ground paigeite with 18% of multi-sulfur iron sodium additive by mass ratio for agglomeration, drying the obtained agglomerate, and reducing and roasting by adopting brown coal as a reducing agent at the roasting temperature of 1100 ℃ for 60 min. Compared with the method without adding the desulphurization slag, the average grain diameter of the metallic iron grains in the roasted ore is increased from 8.5 mu m to 58 mu m, and the subsequent iron and boron separation effect can be effectively improved. The iron grade of the magnetic concentrate is 94.7 percent, B2O3The content is 0.4%, the iron recovery rate is 95.9%, and the boron dissolution rate is 95.2%.
Comparative example 7
The other conditions were the same as in example 4 except that the sodium iron polysulfide additive was used in an amount of 3%; the iron grade of the magnetic concentrate is 90.2 percent, B2O3The content is 0.6%, the iron recovery rate is 91.9%, and the boron dissolution rate is 82.3%.
Comparative example 8
The other conditions were the same as in example 4 except that the sodium iron polysulfide additive was used in an amount of 35%; the iron grade of the magnetic concentrate is 93.7 percent, B2O3The content is 0.3%, the iron recovery rate is 88.3%, and the boron dissolution rate is 85.2%.
Example 5:
the TFe content of a niobium iron ore is 31.9%, Nb2O5The content is 2.9 percent, the milled niobium-iron ore and 15 percent of multi-sulfur iron sodium additive are mixed uniformly and agglomerated, the obtained agglomerate is dried and then is reduced and roasted by adopting anthracite as a reducing agent, the roasting temperature is 1100 ℃, and the roasting time is 120 min. Compared with the method without adding the desulphurization slag, the average grain diameter of the metallic iron grains in the roasted ore is increased from 6.9 mu m to 45 mu m, and the subsequent iron and niobium separation effect can be effectively improved. The iron grade of the magnetic concentrate is 89.6 percent and Nb2O5The content was 0.52%, the iron recovery was 91.5%, and the niobium removal rate was 91.8%.
Comparative example 9
The other conditions were the same as in example 5 except that the sodium iron polysulfide additive was used in an amount of 3%; the iron grade of the magnetic concentrate is 79.2 percent and Nb2O5The content was 1.02%, the iron recovery was 73.5%, and the niobium removal rate was 57.8%.
Comparative example 10
The other conditions were the same as in example 5 except that the sodium iron polysulfide additive was used in an amount of 35%; the iron grade of the magnetic concentrate is 91.9 percent and Nb2O5The content was 0.62%, the iron recovery was 92.8%, and the niobium removal rate was 90.1%.
Attached table: the refractory iron ore of each embodiment is reduced and separated quickly at low temperature
Claims (7)
1. An application method of an additive for strengthening low-temperature rapid reduction of refractory iron ore is characterized in that: the additive contains NaFeS2(ii) a The dosage of the additive is 5-30% of the mass of the iron ore difficult to treat, and the additive is finely ground to be below 100 meshes and then used in a matching way;
mixing iron ore difficult to treat and an additive uniformly for agglomeration, drying the obtained agglomerate, placing the dried agglomerate in a reducing atmosphere for roasting at the roasting temperature of 1000-1100 ℃ for 60-120 min, and grinding and magnetically separating the cooled roasted product to obtain a magnetic metal iron/iron alloy product and nonmagnetic tailings.
2. The method for applying the additive for strengthening the low-temperature rapid reduction of the refractory iron ore according to claim 1, wherein the additive comprises the following components in percentage by weight: the main component of the additive is sodium iron polysulfide and/or hydrated sodium iron polysulfide.
3. The method for applying the additive for strengthening the low-temperature rapid reduction of the refractory iron ore according to claim 1, wherein the additive comprises the following components in percentage by weight: the desulfurization slag generated in the process of producing alumina by the Bayer process of the high-sulfur bauxite, the desulfurization slag generated in the process of recovering the lead-acid battery by the alkali fusion process and the desulfurization slag containing sodium iron polysulfide generated in the smelting process of other nonferrous metals can be directly used as the additive.
4. The application method of the additive for strengthening the low-temperature rapid reduction of the refractory iron ore according to claim 1, characterized in that: further separating and extracting sodium, iron and sulfur components from the nonmagnetic tailings.
5. The application method of the additive for strengthening the low-temperature rapid reduction of the refractory iron ore according to claim 1, characterized in that: after the calcination, the average particle size of the obtained magnetic metallic iron/iron alloy product is greater than or equal to 45 μm.
6. The application method of the additive for strengthening the low-temperature rapid reduction of the refractory iron ore according to claim 1, characterized in that: when the iron ore does not comprise the laterite-nickel ore, the recovery rate of iron is more than or equal to 91 percent after the iron ore is treated by adding the additive;
when the iron ore is the laterite-nickel ore, the recovery rate of Ni is more than or equal to 92 percent after the additive is added to treat the iron ore.
7. The application method of the additive for strengthening the low-temperature rapid reduction of the refractory iron ore according to claim 1, characterized in that:
when the iron ore contains boron, the dissolution rate of the boron is more than or equal to 92 percent after the iron ore is treated by adding the additive;
when the iron ore contains niobium, the removal rate of the Nb is more than or equal to 90 percent after the iron ore is treated by adding the additive;
when the iron ore contains phosphorus, the removal rate of P is more than or equal to 90 percent after the iron ore is treated by adding the additive.
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