Low-sulfur ilmenite beneficiation process and method for preparing high-purity iron from the ilmenite

Abstract

The application discloses a low-sulfur ilmenite beneficiation separation process and a method for preparing high-purity iron by using the ilmenite, and belongs to the technical field of mineral processing and metallurgy. A raw material with TiO2 grade of 18-20% is added with a flotation reagent H2SO4, butyl xanthate and a foaming agent for flotation desulfurization, the desulfurization tailings are subjected to four times of scavenging desulfurization, and the reagent added in each scavenging desulfurization is butyl xanthate and a foaming agent; the desulfurization tailings are subjected to flotation titanium selection to obtain titanium concentrate and titanium tailings. The titanium concentrate is subjected to electric furnace smelting to obtain high-titanium slag and molten iron; and the molten iron is subjected to vacuum refining to obtain high-purity iron. The application reduces the content of harmful elements S, Co, Ni and Cu in the ilmenite as much as possible from the smelting raw material end by combining mineral processing and smelting, thereby reducing the difficulty of subsequent smelting treatment, achieving the technical target of effectively separating the ilmenite, and further meeting various industrial high-end requirements.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of mineral processing and metallurgy, and particularly relates to a low-sulfur ilmenite beneficiation process and a method for preparing high-purity iron by using the ilmenite. BACKGROUND

[0002] Industrial pure iron refers to an iron alloy with an iron content of not less than 99.5% and a carbon content of not higher than 0.04%. Due to its low coercivity, strong corrosion resistance, high toughness, and good heat conduction and soft magnetic properties, the application range of the industrial pure iron is very wide, and the industrial pure iron is often used in the production and manufacturing of precision alloys, electrothermal alloys, high-temperature alloys, clean steels, and the like. With the development and progress of social science and technology, the market demand for the industrial pure iron in China is increasing, and the industrial pure iron has obvious development advantages and a very broad future under the encouragement and support of national policies.

[0003] At present, the traditional process is mainly used to smelt the industrial pure iron in China, and impurities need to be removed through multiple processes, so that the process is complex, the production cost is high, the production difficulty is great, the emission of sulfides and nitrogen oxides is high, the influence on the environment is large, and the composition is difficult to control in the smelting process, which requires high operation requirements and limits the development of the industrial pure iron production technology in China.

[0004] The preparation of high-purity iron from the titanium slag by-product molten iron can increase the added value of the titanium slag by-product molten iron and improve the economic benefits of enterprises, but the higher the contents of S, Co, Ni and Cu in the titanium concentrate, the higher the contents of S, Co, Ni and Cu in the titanium slag by-product molten iron, which will affect the technical and economic indicators of the subsequent production of high-purity iron. SUMMARY

[0005] In order to overcome the defects of the prior art, the application reduces the contents of harmful elements S, Co, Ni and Cu from the smelting raw material end as much as possible, so as to reduce the difficulty of subsequent smelting treatment.

[0006] To achieve the above-mentioned application purposes, the application provides a low-sulfur ilmenite beneficiation process and a method for preparing high-purity iron by using the ilmenite, which comprises the following steps:

[0007] ① The low-sulfur ilmenite raw material is subjected to flotation desulfurization (desulfurization roughing) to obtain desulfurization tailings I and sulfur rough concentrate; the flotation desulfurization process adds H2SO4, butyl xanthate and a foaming agent (commonly referred to as 2# oil in the industry);

[0008] ② The desulfurization tailings I obtained in step ① are subjected to scavenging desulfurization to obtain desulfurization tailings II and sulfur scavenging concentrate; the scavenging process adds butyl xanthate at an amount of 75 g / t and a foaming agent at an amount of 16 g / t;

[0009] ③The desulfurization tailings II obtained in step 2 is subjected to the second desulfurization by scavenging to obtain desulfurization tailings III and the second sulfur scavenging concentrate; the reagent addition amount in the scavenging process is butyl xanthate 75 g / t and frother 16 g / t;

[0010] ④The desulfurization tailings III obtained in step 3 is subjected to the third desulfurization by scavenging to obtain desulfurization tailings IV and the third sulfur scavenging concentrate; the reagent addition amount in the scavenging process is butyl xanthate 75 g / t and frother 16 g / t;

[0011] ⑤The desulfurization tailings IV obtained in step 4 is subjected to the fourth desulfurization by scavenging to obtain desulfurization tailings V and the fourth sulfur scavenging concentrate; the reagent addition amount in the scavenging process is butyl xanthate 75 g / t and frother 16 g / t;

[0012] ⑥The desulfurization tailings V obtained in step 5 is subjected to the titanium flotation (titanium roughing) to obtain the first titanium flotation concentrate and the titanium tailings; the titanium collector addition amount is 1800 g / t; the adjusting agent is sulfuric acid, and the sulfuric acid addition amount is 800 g / t;

[0013] ⑦The first titanium flotation concentrate obtained in step 6 is subjected to the titanium flotation to obtain the second titanium flotation concentrate and the titanium tailings A; the titanium adjusting agent is sulfuric acid, and the sulfuric acid addition amount is 150 g / t;

[0014] ⑧The second titanium flotation concentrate obtained in step 7 is subjected to the titanium flotation to obtain the titanium concentrate and the titanium tailings B; the titanium adjusting agent is sulfuric acid, and the sulfuric acid addition amount is 100 g / t;

[0015] ⑨The titanium concentrate obtained in step 8 is subjected to the electric furnace smelting to obtain the high-titanium slag and the molten iron;

[0016] ⑩The molten iron obtained in step 9 is subjected to the vacuum refining to obtain the high-purity iron; the refining vacuum degree is 3 Pa, the refining time is 40 min, and the refining temperature is 1590 ℃.

[0017] In the technical scheme, further, the TiO2 grade of the low-sulfur titanium-iron ore raw material in step 1 is 18-20%; the frother in step 1 is C8-C10 normal iso-aliphatic dihydric alcohol, the frother addition amount is 50 g / t, the H2SO4 addition amount is 800 g / t, and the butyl xanthate addition amount is 300 g / t.

[0018] In the technical scheme, further, the titanium tailings A in step 7 is returned to step 6 and mixed with the desulfurization tailings V to be subjected to the titanium flotation again.

[0019] In the technical scheme, further, the titanium tailings B in step 7 is returned to step 6 and mixed with the first titanium flotation concentrate to be subjected to the titanium flotation again.

[0020] Compared with the prior art, the beneficial effects of the present application are:

[0021] The application reduces the content of harmful elements S, Co, Ni and Cu in ilmenite as much as possible from the end of smelting raw materials by combining beneficiation and smelting, thereby reducing the difficulty of subsequent smelting treatment, realizing effective separation of ilmenite, and achieving industrial demand. BRIEF DESCRIPTION OF DRAWINGS

[0022] Figure 1 The process flow chart of the application. DETAILED DESCRIPTION

[0023] The application will be further described below in conjunction with specific examples, but the application is not limited in any way by the examples. For the sake of brevity, the raw materials in the following examples are all commercially available products unless otherwise specified, and the methods used are all conventional methods unless otherwise specified. The chemical composition of the low-sulfur ilmenite raw material in the examples is shown in Table 1, and the titanium collection agent MOH is produced by Hubei Shishou Jingjiang Beneficiation Reagent Co., Ltd. The detection of the chemical composition of the raw material, titanium concentrate and high-purity iron is based on the standards YS / T 360-2011 "Chemical Analysis Method of Ilmenite Concentrate", GB / T 6730.76-2017 "Determination of Potassium, Sodium, Vanadium, Copper, Zinc, Lead, Chromium, Nickel, Cobalt Content in Iron Ore by Inductively Coupled Plasma Atomic Emission Spectrometry", YS / T 351-2015 "Ilmenite Concentrate", SN / T 4020-2013 "Determination of Impurity Content in Pure Iron by X-ray Fluorescence Spectrometry", etc.

[0024] Table 1 Chemical composition of raw material (%)

[0025] Name TiO2 TFe Co Ni Cu S Run-of-mine 18.57 13.38 0.021 0.018 0.015 0.570

[0026] Example 1

[0027] A low-sulfur ilmenite beneficiation and separation process and a method for preparing high-purity iron using the ilmenite, comprising the following steps:

[0028] ① The low-sulfur ilmenite raw material is subjected to flotation desulfurization (desulfurization roughing) to obtain desulfurization tailings I and sulfur rough concentrate. The flotation reagents added in the flotation desulfurization process are H2SO4, butyl xanthate and a foaming agent (2# oil);

[0029] ② The desulfurization tailings I obtained in step ① are subjected to scavenging and desulfurization to obtain desulfurization tailings II and sulfur scavenging concentrate. The reagents added in the scavenging process are butyl xanthate 75 g / t and a foaming agent 16 g / t;

[0030] ③ The desulfurization tailings II obtained in step ② are subjected to scavenging and desulfurization to obtain desulfurization tailings III and sulfur scavenging concentrate. The reagents added in the scavenging process are butyl xanthate 75 g / t and a foaming agent 16 g / t;

[0031] IV and sulfur sweep four concentrate; the reagent added in the sweeping process is butyl xanthate 75 g / t, and the frother is 16 g / t;

[0032] IV and sulfur sweep four concentrate; the reagent added in the sweeping process is butyl xanthate 75 g / t, and the frother is 16 g / t;

[0033] V is carried out for titanium flotation (titanium roughing flotation), to obtain titanium flotation concentrate 1 and titanium tailings; the titanium collector is MOH, and the adjusting agent is sulfuric acid; the collector is added in an amount of 1800 g / t, and the sulfuric acid is added in an amount of 800 g / t;

[0034] V is carried out for titanium flotation (titanium roughing flotation), to obtain titanium flotation concentrate 1 and titanium tailings; the titanium collector is MOH, and the adjusting agent is sulfuric acid; the collector is added in an amount of 1800 g / t, and the sulfuric acid is added in an amount of 800 g / t;

[0035] V is carried out for titanium flotation (titanium roughing flotation), to obtain titanium flotation concentrate 1 and titanium tailings; the titanium collector is MOH, and the adjusting agent is sulfuric acid; the collector is added in an amount of 1800 g / t, and the sulfuric acid is added in an amount of 800 g / t;

[0036] Table 2: Multi-element chemical composition analysis results of titanium concentrate (%)

[0037] Name TiO2 TFe Co Ni Cu S Titanium concentrate 47.36 32.40 ＜0.01 ＜0.01 ＜0.01 0.033

[0038] V is carried out for titanium flotation (titanium roughing flotation), to obtain titanium flotation concentrate 1 and titanium tailings; the titanium collector is MOH, and the adjusting agent is sulfuric acid; the collector is added in an amount of 1800 g / t, and the sulfuric acid is added in an amount of 800 g / t;

[0039] V is carried out for titanium flotation (titanium roughing flotation), to obtain titanium flotation concentrate 1 and titanium tailings; the titanium collector is MOH, and the adjusting agent is sulfuric acid; the collector is added in an amount of 1800 g / t, and the sulfuric acid is added in an amount of 800 g / t;

[0040] The TiO2 grade of the low-sulfur titanomagnetite raw material in step ① is 18-20%; the frother in step ① is C8-C10 normal and iso-aliphatic dihydric alcohol, the frother is added in an amount of 50 g / t; the H2SO4 is added in an amount of 800 g / t, and the butyl xanthate is added in an amount of 300 g / t.

[0041] The titanium tailings A in step ⑦ is returned to step ⑥ and mixed with the desulfurization tailings V for re-titanium flotation. The titanium tailings B in step ⑧ is returned to step ⑦ and mixed with the titanium flotation concentrate 1 for re-titanium flotation.

[0042] Table 3: Chemical composition of high-purity iron (%)

[0043] Name C Ti Co Ni Cu S P Al High purity iron 0.002 0.001 0.0005 0.0007 0.0005 0.002 0.005 0.005

[0044] Comparative Example 1

[0045] The non-deep desulfurization titanium concentrate is taken from a titanium concentrator in Panzhihua, and its chemical composition is shown in Table 4:

[0046] Table 4 Chemical composition analysis results of non-deep desulfurization titanium concentrate

[0047] Name TiO2 TFe Co Ni Cu S Titanium concentrate 46.95 31.89 0.019 0.012 0.011 0.191

[0048] 1. The above titanium concentrate is subjected to electric furnace smelting to obtain high-titanium slag and molten iron;

[0049] 2. The above molten iron is subjected to vacuum refining to obtain high-purity iron; the refining vacuum is 3 Pa, the refining time is 40 min, and the refining temperature is 1590℃. The chemical composition analysis results of the prepared high-purity iron are shown in Table 5:

[0050] Table 5 Chemical composition analysis results of high-purity iron prepared from non-deep desulfurization titanium concentrate

[0051] Name C Ti Co Ni Cu S P Al High purity iron 0.002 0.001 0.0011 0.009 0.0012 0.003 0.005 0.005

[0052] For any person skilled in the art, many possible changes and modifications, or equivalent embodiments of equivalent changes can be made to the technical solutions of the present application by using the disclosed technical contents without departing from the scope of the technical solutions of the present application. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present application should still belong to the scope of protection of the technical solutions of the present application.

Claims

1. A low-sulfur ilmenite beneficiation process and a method for preparing high-purity iron using the ilmenite, characterized by, The method comprises the following steps: ① low-sulfur ilmenite raw material is subjected to flotation desulfurization to obtain desulfurization tailings I and sulfur rough concentrate; the flotation reagent added in the process of flotation desulfurization is H2SO4, butyl xanthate and a foaming agent; the TiO2 grade of the low-sulfur ilmenite raw material is 18%-20%; the foaming agent is C8-C10 normal and iso-aliphatic dihydric alcohol, the foaming agent is added in an amount of 50 g / t, H2SO4 is added in an amount of 800 g / t, and butyl xanthate is added in an amount of 300 g / t; ② the desulfurization tailings I obtained in step ① are subjected to scavenging desulfurization to obtain desulfurization tailings II and sulfur scavenging concentrate; the reagent is added in an amount of 75 g / t of butyl xanthate and 16 g / t of foaming agent in the process of scavenging; ③ the desulfurization tailings II obtained in step ② are subjected to scavenging desulfurization to obtain desulfurization tailings III and sulfur scavenging concentrate; the reagent is added in an amount of 75 g / t of butyl xanthate and 16 g / t of foaming agent in the process of scavenging; ④ the desulfurization tailings III obtained in step ③ are subjected to scavenging desulfurization to obtain desulfurization tailings IV and sulfur scavenging concentrate; the reagent is added in an amount of 75 g / t of butyl xanthate and 16 g / t of foaming agent in the process of scavenging; ⑤ the desulfurization tailings IV obtained in step ④ are subjected to scavenging desulfurization to obtain desulfurization tailings V and sulfur scavenging concentrate; the reagent is added in an amount of 75 g / t of butyl xanthate and 16 g / t of foaming agent in the process of scavenging; ⑥ the desulfurization tailings V obtained in step ⑤ are subjected to flotation titanium selection to obtain titanium flotation concentrate 1 and titanium tailings; the titanium selection collector is added in an amount of 1800 g / t, diesel oil is added in an amount of 600 g / t, and the adjusting agent is sulfuric acid, which is added in an amount of 800 g / t; ⑦ the titanium flotation concentrate 1 obtained in step ⑥ is subjected to flotation titanium selection to obtain titanium flotation concentrate 2 and titanium tailings A; the titanium selection adjusting agent is sulfuric acid, which is added in an amount of 150 g / t; the titanium tailings A obtained in step ⑦ is mixed with the desulfurization tailings V and subjected to re-flotation titanium selection; ⑧ the titanium flotation concentrate 2 obtained in step ⑦ is subjected to flotation titanium selection to obtain titanium concentrate and titanium tailings B; the titanium selection adjusting agent is sulfuric acid, which is added in an amount of 100 g / t; the titanium tailings B obtained in step ⑧ is mixed with the titanium flotation concentrate 1 and subjected to re-flotation titanium selection; ⑨ the titanium concentrate obtained in step ⑧ is subjected to electric furnace smelting to obtain high-titanium slag and molten iron; ⑩ the molten iron obtained in step ⑨ is subjected to vacuum refining to obtain high-purity iron; the refining vacuum degree is 3 Pa, the refining time is 40 min, and the refining temperature is 1590 ℃.

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