Process for directly producing fluidized chlorination furnace charge from ilmenite concentration-electric furnace smelting

Abstract

The application discloses a process for preparing a fluidized chlorination furnace charge by ilmenite concentrate concentration and electric furnace smelting, which comprises the following steps: S1, analyzing the element distribution state of ilmenite concentrates from different regions, and selecting ilmenite concentrates with magnesium element content in ilmenite phase lower than 0.5% as raw materials for concentration; S2, removing impurities by concentration after grinding treatment of the ilmenite concentrates selected in S1 to obtain high-quality titanium concentrate; and S3, smelting the high-quality titanium concentrate obtained in S2 by an electric furnace to obtain high-titanium slag meeting the requirements of the fluidized chlorination furnace charge. The high-titanium slag obtained by smelting the high-quality titanium concentrate by the electric furnace does not need to be subjected to impurity removal treatment, and qualified fluidized chlorination furnace charge can be obtained, the beneficiation method for removing impurities is low in cost and short in process, the safe supply of raw materials for the fluidized chlorination production of China is ensured, and the process has important significance for promoting the development of the titanium industry of China.

Description

TECHNICAL FIELD

[0001] The application belongs to the field of utilization of ilmenite, and particularly relates to a process for directly preparing boiling chlorination furnace charge through ilmenite concentration-electric furnace smelting. BACKGROUND

[0002] Currently, the method for preparing boiling chlorination furnace charge from titanium concentrate is mainly to smelt high-titanium slag from titanium concentrate and then perform impurity removal treatment, such as the Canadian UGS slag preparation process, which has problems of long process, large acid consumption, high cost, and serious pollution, and therefore, in view of the problems of long process and high cost in the current preparation of boiling chlorination furnace charge from titanium concentrate, the purpose of the present application is to provide a process for directly preparing boiling chlorination furnace charge through ilmenite concentration-electric furnace smelting. SUMMARY

[0003] In view of the problems of long process and high cost in the current preparation of boiling chlorination furnace charge from titanium concentrate, the purpose of the present application is to provide a process for preparing boiling chlorination furnace charge through ilmenite concentration-electric furnace smelting.

[0004] The present application provides the following technical solution: a process for preparing boiling chlorination furnace charge through ilmenite concentration-electric furnace smelting, comprising the following steps:

[0005] S1, analyzing the element distribution state of ilmenite concentrate from different regions, and selecting ilmenite concentrate with a magnesium element mass percentage content of less than 0.5% in the ilmenite phase as the raw material for subsequent concentration;

[0006] S2, performing concentration and impurity removal on the ilmenite concentrate selected in S1 after grinding treatment to obtain high-quality titanium concentrate; the mass percentage content of MgO in the high-quality titanium concentrate is less than or equal to 0.5%;

[0007] S3, smelting the high-quality titanium concentrate obtained in S2 by using an electric furnace to obtain high-titanium slag meeting the requirements of boiling chlorination furnace charge.

[0008] Preferably, the analysis method of the element distribution state of ilmenite includes one or more of scanning electron microscopy-energy spectrum analysis, electron probe, etc.

[0009] In the present application, the ilmenite with a magnesium element content of less than 0.5% in the ilmenite phase includes ilmenite concentrate with an average magnesium element mass percentage content of less than 0.5% in the non-gangue component. The present application first proposes the ilmenite with a magnesium element content of less than 0.5% in the ilmenite phase as the preliminary raw material screening basis, and the high-titanium slag meeting the requirements of boiling chlorination furnace charge can be quickly obtained through subsequent concentration and impurity removal. Meanwhile, the present application provides a necessary condition for quickly and stably obtaining the high-titanium slag meeting the requirements of boiling chlorination furnace charge from ilmenite concentrate.

[0010] Preferably, the ilmenite grinding method comprises one or more of ball milling, high-pressure roller milling, wet milling, and vertical milling; and the ilmenite cleaning method comprises one or more of magnetic separation, flotation, and gravity separation.

[0011] Preferably, the cleaning of the ilmenite concentrate S1 comprises: grinding the ilmenite concentrate S1 by a ball mill to a -200 mesh content of 70-95%, preferably 90%, and then performing flotation separation by using sodium oleate as a collector at a dosage of 1000-2000 g / t, preferably 1200-1600 g / t, using water glass as a depressor at a dosage of 700-900 g / t, preferably 750-850 g / t, and using sulfuric acid as an adjusting agent at a dosage of 800-1200 g / t, preferably 900-1100 g / t, and further preferably 1000 g / t, to obtain the high-quality ilmenite concentrate.

[0012] Preferably, the cleaning of the ilmenite concentrate S1 comprises: grinding the ilmenite concentrate S1 by a ball mill to a -200 mesh content of 70-95%, preferably 90%, and then performing high-gradient magnetic separation by using a high-gradient magnetic separator at a magnetic field strength of 0.2-0.5 T, a vertical ring rotating speed of 5.5-6.5 r / min, preferably 6.0 r / min, a stroke of 11-13 mm, preferably 12 mm, and a stroke frequency of 90-110 r / min, preferably 100 r / min, to obtain the high-quality ilmenite concentrate.

[0013] Preferably, the high-quality ilmenite concentrate S2 has a mass percentage of TiO2≥46%, SiO2≤1.4%, MgO≤0.5%, and CaO≤0.18%. In the present application, the MgO content in the high-quality ilmenite concentrate must be strictly controlled to be ≤0.5 wt%, otherwise, the MgO content in the titanium slag S3 will be greatly increased, which will result in that the product obtained after the electric furnace smelting cannot be directly used for the production of boiling chlorination.

[0014] Preferably, the electric furnace smelting in S3 is performed at a temperature of 1600-1750℃ for 1-3 hours.

[0015] Preferably, the high-titanium slag obtained after the electric furnace smelting has a mass percentage of TiO2≥85%, SiO2≤2.5%, MgO≤1.0%, and CaO≤0.35%.

[0016] The present application has the following advantages:

[0017] The titanium concentrate is first selected and then smelted by an electric furnace to directly prepare a process meeting the requirements of boiling chlorination, the invention first attempts to select the ilmenite with the mass percentage of magnesium element in the ilmenite phase being lower than 0.5% as the target mineral according to the mineral phase element distribution of ilmenite resources in different mining areas, and then adopts the re-selection method to separate and remove impurities to MgO≤0.5wt%, so as to obtain the high-quality ilmenite concentrate with low calcium and magnesium, the high-titanium slag obtained by smelting the high-quality ilmenite concentrate by the electric furnace does not need to be treated by removing impurities, and can be used as qualified boiling chlorination furnace charge, the cost of removing impurities by the beneficiation method is low, and the process is short. BRIEF DESCRIPTION OF DRAWINGS

[0018] Figure 1 SEM-EDS diagram of the raw material ilmenite concentrate used in examples 1 and 2. DETAILED DESCRIPTION

[0019] The specific embodiments of the invention will be further illustrated by the following examples, but the specific embodiments of the invention are not limited to the following examples.

[0020] In the examples of the invention, the main chemical component content of the raw material ilmenite concentrate is (wt%): TiO2: 44.86%, SiO2: 3.32%, CaO: 1.32%, MgO: 1.45%, and the balance is iron, aluminum, manganese and other common oxides in ilmenite. In the raw material used, the content of magnesium oxide in gangue is greater than 1.45%.

[0021] Example 1

[0022] A process for preparing boiling chlorination furnace charge by ilmenite concentrate selection-electric furnace smelting, comprising the following steps:

[0023] S1, using scanning electron microscopy-energy spectrum analysis to analyze the mineral phase of the obtained ilmenite concentrate, Figure 1 The SEM-EDS diagram of the ilmenite concentrate used in the example, EDS points 54 and 58 are the ilmenite phase element composition, and it can be seen that the content of Mg element is 0.15% and 0.05%, which can be used for the next step of separation and utilization.

[0024] S2, grinding the ilmenite concentrate selected in S1 by a ball mill for 10 min, the -200 mesh content reaches 90.12%, and the flotation is used for separation and removal of impurities, the collector sodium oleate 1500g / t is selected, the depressor water glass 800g / t is used, and the regulator sulfuric acid 1000g / t is used, the TiO2 in the high-quality ilmenite concentrate obtained is 47.26%, the SiO2 is 0.92%, the CaO is 0.16%, the MgO is 0.41%, the recovery rate of titanium is 85.69%, and the yield of high-quality ilmenite concentrate is 82.16%.

[0025] S3 The high-titanium slag TiO2: 89.26%, TFe: 4.89%, SiO2: 1.98%, CaO: 0.31%, MgO: 0.79% obtained by smelting the high-quality titanium concentrate obtained in S2 in an electric furnace at a smelting temperature of 1700 DEG C and a smelting time of 2 hours can meet the requirements of the boiling chlorination furnace charge.

[0026] After selecting the ilmenite concentrate with the mass percentage of magnesium element in the ilmenite phase being less than 0.5% as the raw material for subsequent cleaning, the above steps S2 and S3 are repeated to continuously produce more than 100 tons of high-titanium slag meeting the requirements of the boiling chlorination furnace charge.

[0027] Example 2

[0028] A process for preparing a boiling chlorination furnace charge by cleaning ilmenite concentrate in an electric furnace, comprising the following steps:

[0029] S1 The obtained titanium concentrate is subjected to mineral phase analysis by scanning electron microscopy-energy dispersive spectroscopy, Figure 1 The SEM-EDS diagram of the ilmenite concentrate used in the example shows that the contents of Mg element in the ilmenite phase elements of EDS points 54 and 58 are 0.15% and 0.05% respectively, which can be used for the next step of separation and utilization.

[0030] S2 The titanium concentrate selected in S1 is ground for 10 minutes by a ball mill to obtain a -200 mesh content of 90.12%, and then subjected to separation and impurity removal by a high gradient magnetic separator at a magnetic field strength of 0.3 T, a vertical ring rotating speed of 6.0 r / min, a stroke of 12 mm, and a stroke frequency of 100 r / min, to obtain high-quality titanium concentrate with TiO2: 47.08%, SiO2: 1.02%, CaO: 0.17%, and MgO: 0.45%, and a titanium recovery rate of 80.12%, and a yield of high-quality titanium concentrate of 75.56%.

[0031] S3 The high-quality titanium concentrate obtained in S2 is smelted in an electric furnace at a smelting temperature of 1750 DEG C and a smelting time of 1 hour to obtain high-titanium slag TiO2: 87.15%, TFe: 4.95%, SiO2: 2.11%, CaO: 0.33%, MgO: 0.92%, which can meet the requirements of the boiling chlorination furnace charge.

[0032] After selecting the ilmenite concentrate with the mass percentage of magnesium element in the ilmenite phase being less than 0.5% as the raw material for subsequent cleaning, the above steps S2 and S3 are repeated to continuously produce more than 100 tons of high-titanium slag meeting the requirements of the boiling chlorination furnace charge.

[0033] Comparative Example 1

[0034] Other conditions and example 1 are consistent, the difference is that the raw material titanium concentrate is smelted by electric furnace, smelting temperature is 1700 DEG C, smelting time is 2 hours, high titanium slag TiO2: 76.85%, TFe: 5.23%, SiO2: 6.52%, CaO: 2.64%, MgO: 2.89%, unable to meet the requirement of boiling chlorination furnace charge.

[0035] Comparative example 2

[0036] Other conditions and example 1 are consistent, the difference is that the raw material titanium concentrate is smelted by electric furnace, smelting temperature is 1700 DEG C, smelting time is 2 hours, high titanium slag TiO2: 76.85%, TFe: 5.23%, SiO2: 6.52%, CaO: 2.64%, MgO: 2.89%, unable to meet the requirement of boiling chlorination furnace charge.

[0037] The raw material ilmenite concentrate is ground by ball mill for 10 min, and flotation is used for separation and impurity removal, the selective collector sodium oleate is 500 g / t, the depressor is water glass 600 g / t, and the regulator is hydrochloric acid 300 g / t, the TiO2 in the obtained titanium concentrate is 46.12%, SiO2 is 1.56%, CaO is 0.35%, MgO is 0.89%, the recovery rate of titanium is 70.23%, and the yield of high-quality titanium concentrate is 75.63%.

[0038] S2 is obtained by smelting the high-quality titanium concentrate of S1 by electric furnace, smelting temperature is 1700 DEG C, smelting time is 2 hours, high titanium slag TiO2: 82.23%, TFe: 4.96%, SiO2: 3.11%, CaO: 0.72%, MgO: 1.66%, unable to meet the requirement of boiling chlorination furnace charge.

[0039] The above only describes the preferred embodiments of the present application, and the protection scope of the present application is not limited to the above examples. For those skilled in the art, the improvements and changes obtained without departing from the technical concept of the present application should also be considered as the protection scope of the present application.

Claims

1. A process for the production of fluid bed chlorination feed material from ilmenite concentrate by beneficiation-electric furnace smelting, characterised in that, The method comprises the following steps: S1. Analyzing the element distribution state of ilmenite concentrates from different regions, and selecting ilmenite concentrates with a magnesium element mass percentage in ilmenite phase of less than 0.5% as raw materials for cleaning; S2. Cleaning the ilmenite concentrates selected in S1 after grinding treatment to obtain high-quality titanium concentrates; the mass percentage of MgO in the high-quality titanium concentrates is ≤0.5%; The cleaning includes: grinding the ilmenite concentrates selected in S1 by a ball mill for 8-15 min, and separating and cleaning by flotation, selecting a sodium oleate collector at 1200-1700 g / t, a water glass inhibitor at 700-900 g / t, and a hydrochloric acid regulator at 800-1200 g / t to obtain the high-quality titanium concentrates; S3. Smelting the high-quality ilmenite concentrates obtained in S2 by an electric furnace to obtain high-titanium slag meeting the requirements of a boiling chlorination furnace; in S3, the temperature of the electric furnace smelting is 1600-1750°C, and the smelting time is 1-3 hours.

2. A process for the preparation of fluid bed chlorination feed from ilmenite concentrate by beneficiation-ilmenite electric furnace smelting according to claim 1, characterized by: The analysis method of the element distribution state of ilmenite includes one or more of scanning electron microscopy-energy spectrum analysis and electron probe.

3. A process for the preparation of fluid bed chlorination feed material from ilmenite concentrate by beneficiation and electric furnace smelting according to claim 1 characterised in that: The ilmenite with a magnesium element content in ilmenite phase of less than 0.5% includes ilmenite concentrates with an average mass percentage of magnesium element in non-gangue components of less than 0.5%.

4. A process for the preparation of fluid bed chlorination feed material from ilmenite concentrate by beneficiation and electric furnace smelting according to claim 1 characterised in that: The cleaning includes: grinding the ilmenite concentrates selected in S1 by a ball mill for 10 min, and separating and cleaning by flotation, selecting a sodium oleate collector at 1400-1600 g / t, a water glass inhibitor at 750-850 g / t, and a hydrochloric acid regulator at 900-1100 g / t to obtain the high-quality titanium concentrates.

5. A process for the preparation of fluid bed chlorination feed material from ilmenite concentrate by beneficiation and electric furnace smelting as claimed in claim 1, wherein: In the high-quality titanium concentrates obtained in S2, the mass percentages of TiO2, SiO2, MgO, and CaO are ≥46%, ≤1.4%, ≤0.5%, and ≤0.18%, respectively.

6. A process for the preparation of fluid bed chlorination feed material from ilmenite concentrate by beneficiation and electric furnace smelting according to claim 1 characterised in that: In S3, the temperature of the electric furnace smelting is 1600-1750°C, and the smelting time is 1-3 hours.

7. A process for the preparation of fluid bed chlorination feed material from ilmenite concentrate by beneficiation and electric furnace smelting according to claim 1 characterised in that: In the high-titanium slag obtained after smelting by the electric furnace, the mass percentages of TiO2, SiO2, MgO, and CaO are ≥85%, ≤2.5%, ≤1.0%, and ≤0.35%, respectively.

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