CN116082026A - Preparation process of ilmenite and method for inhibiting perovskite from generating in sintering process - Google Patents
Preparation process of ilmenite and method for inhibiting perovskite from generating in sintering process Download PDFInfo
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- CN116082026A CN116082026A CN202211564131.3A CN202211564131A CN116082026A CN 116082026 A CN116082026 A CN 116082026A CN 202211564131 A CN202211564131 A CN 202211564131A CN 116082026 A CN116082026 A CN 116082026A
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- ilmenite
- raw materials
- perovskite
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- magnetite
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- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000005245 sintering Methods 0.000 title claims abstract description 23
- 230000002401 inhibitory effect Effects 0.000 title claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 40
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 19
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 19
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 18
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 17
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000292 calcium oxide Substances 0.000 claims abstract description 17
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 17
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 17
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 17
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims 1
- 238000003723 Smelting Methods 0.000 abstract description 3
- XUIMIQQOPSSXEZ-IGMARMGPSA-N silicon-28 atom Chemical group [28Si] XUIMIQQOPSSXEZ-IGMARMGPSA-N 0.000 abstract 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 238000003837 high-temperature calcination Methods 0.000 description 5
- 229910001200 Ferrotitanium Inorganic materials 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000002223 garnet Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000002411 adverse Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000004484 Briquette Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2683—Other ferrites containing alkaline earth metals or lead
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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Abstract
The invention discloses a preparation process of ilmenite and a method for inhibiting perovskite from generating in a sintering process, and belongs to the technical field of ilmenite preparation processes. The invention relates to a preparation process of ilmenite, which takes ferric oxide, titanium dioxide, silicon dioxide and calcium oxide as raw materials to synthesize the ilmenite, and the components are controlled to be proportioned according to the following parts by weight: 28-32 parts of ferric oxide, 20-23 parts of titanium dioxide, 15-18 parts of silicon dioxide and 28-32 parts of calcium oxide. According to the invention, the ilmenite can be synthesized by adopting the raw materials with specific components and controlling the mass ratio of the raw materials, and the generation of perovskite is fundamentally inhibited, so that theoretical guidance can be provided for the sintering of the vanadium titano-magnetite, and the smelting quality of the vanadium titano-magnetite is ensured.
Description
Technical Field
The invention belongs to the technical field of ilmenite preparation processes, and particularly relates to a preparation process of ilmenite and a method for inhibiting perovskite generation in a sintering process.
Background
The vanadium titano-magnetite is used as the iron ore resource with reserve and exploitation amount occupying the third place in China, is mainly distributed in the places of Panzhihua-Xichang, hebei Maillard and Shanxi Han, and is an important strategic resource for extracting and utilizing vanadium and titanium. However, vanadium titano-magnetite is difficult to smelt iron ore, and perovskite which is easy to generate in the sintering process can deteriorate the quality index of the sintered ore, and has profound influence on the subsequent steel smelting process. Therefore, the inhibition of perovskite production becomes an important way for strengthening the sintering of vanadium titano-magnetite, and is one of the core actions for improving the utilization of vanadium titano-magnetite.
In industrial production, the aim of controlling the production of perovskite is usually achieved by optimizing the operating regime, but this does not eradicate the production of perovskite from the source. Therefore, how to inhibit the generation of perovskite from the source has important significance for guaranteeing the sintering quality of vanadium titano-magnetite.
Disclosure of Invention
1. Problems to be solved
The invention aims to provide a preparation process of ilmenite and a method for inhibiting perovskite from being generated in a sintering process, so as to inhibit perovskite from being generated in the sintering process of vanadium titano-magnetite, thereby adversely affecting the quality of sintered ores.
2. Technical proposal
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the invention relates to a preparation process of ilmenite, which takes ferric oxide, titanium dioxide, silicon dioxide and calcium oxide as raw materials to synthesize the ilmenite, and the components are controlled to be proportioned according to the following parts by weight:
further, the method specifically comprises the steps of raw material mixing, briquetting and roasting, wherein the roasting temperature is 1000-1250 ℃, and the heat preservation time is 20-30min.
Further, the raw materials of each component are placed in a mechanical mixer to be fully and uniformly mixed for 20-30min when the raw materials are mixed.
Further, the uniformly mixed raw materials are pressed into cylindrical samples with the height of 15-20mm and the diameter of 15-20mm in a tablet press.
Further, the pressing pressure is 8-12Mpa.
Further, the sample after the briquette is directly heated from room temperature to the roasting temperature during roasting.
The method for inhibiting perovskite from generating in the sintering process of vanadium titano-magnetite takes the vanadium titano-magnetite as a main raw material for proportioning, and simultaneously regulates and controls the components of the mixture, and controls the mass parts of ferric oxide, titanium dioxide, silicon dioxide and calcium oxide in the mixture as follows:
furthermore, the sintering temperature of the mixture is controlled to be 1000-1250 ℃ and the sintering time is controlled to be 20-30min.
3. Advantageous effects
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the preparation process of the ilmenite, disclosed by the invention, the ilmenite can be synthesized by adopting the raw materials of specific components and controlling the mass ratio of the raw materials, and the synthetic method can provide theoretical guidance for sintering of the vanadium titano-magnetite, so that the generation of perovskite is fundamentally inhibited, the smelting quality of the vanadium titano-magnetite is ensured, a new thought and angle are provided for the efficient utilization of refractory ores such as the vanadium titano-magnetite, and the purity of the ilmenite sample prepared by the method can be up to more than 90-95%.
(2) According to the method for inhibiting the generation of the perovskite in the sintering process of the vanadium titano-magnetite, the component proportion in the raw materials of the sintering ore is optimally controlled, so that the titanium-containing compound can be converted into other titanium-containing compounds (ilmenite) with less influence on the performance of the sintering ore from the perovskite, and the adverse influence of the generation of the perovskite in the sintering process of the vanadium titano-magnetite can be fundamentally inhibited.
Drawings
FIG. 1 is a flow chart of the process for preparing ilmenite according to the present invention.
Detailed Description
The invention is further described below in connection with specific embodiments.
Example 1
The preparation raw materials of the ilmenite of this embodiment include: the iron oxide, titanium dioxide, silicon dioxide and calcium oxide are prepared from the following raw materials in parts by mass:
the preparation method of the ilmenite comprises the following specific steps:
(1) Mixing the raw materials uniformly
Taking 19g of total mass of ferric oxide, titanium dioxide, silicon dioxide and calcium oxide according to the parts by mass, and fully and uniformly mixing the 19g of total mass in a mechanical mixer for 22min;
(2) Briquetting formation
Pressing the uniformly mixed raw materials into a cylindrical sample with the height of 18mm and the diameter of 17mm in a tablet press under the pressure of 10 Mpa;
(3) High temperature calcination
Heating the pressed cylindrical sample from room temperature to 1200 ℃, and preserving heat at the temperature for 23min;
(4) Purity detection
The sample obtained after high-temperature roasting is subjected to X-ray diffraction phase composition analysis and is compared with standard phase diffraction peak data of ilmenite, and the result shows that: the purity of the ilmenite sample prepared in this example is as high as 97.
Example 2
The preparation raw materials of the ilmenite of this embodiment include: the iron oxide, titanium dioxide, silicon dioxide and calcium oxide are prepared from the following raw materials in parts by mass:
the preparation method of the ilmenite comprises the following specific steps:
(1) Mixing the raw materials uniformly
Taking 17g of total mass of ferric oxide, titanium dioxide, silicon dioxide and calcium oxide according to the parts by mass, and fully and uniformly mixing in a mechanical mixer for 20min;
(2) Briquetting formation
Pressing the uniformly mixed raw materials into a cylindrical sample with the height of 17mm and the diameter of 15mm in a tablet press under the pressure of 10 Mpa;
(3) High temperature calcination
Heating the pressed cylindrical sample from room temperature to 1100 ℃, and preserving heat at the room temperature for 25min;
(4) Purity detection
And (3) carrying out X-ray diffraction phase composition analysis on the sample obtained after high-temperature roasting, and comparing the sample with standard phase diffraction peak data of ilmenite. The results show that: the purity of the ferrotitanium sample prepared by the method is up to 95%.
Example 3
The preparation raw materials of the ilmenite of this embodiment include: the iron oxide, titanium dioxide, silicon dioxide and calcium oxide are prepared from the following raw materials in parts by mass:
the preparation method of the ilmenite comprises the following specific steps:
(1) Mixing the raw materials uniformly
Taking 20g of total mass of ferric oxide, titanium dioxide, silicon dioxide and calcium oxide according to the parts by mass, and fully and uniformly mixing the 20g of total mass in a mechanical mixer for 25min;
(2) Briquetting formation
Pressing the uniformly mixed raw materials into a cylindrical sample with the height of 20mm and the diameter of 18mm in a tablet press under the pressure of 8 Mpa;
(3) High temperature calcination
Heating the pressed cylindrical sample from room temperature to 1250 ℃, and preserving heat at the room temperature for 20min;
(4) Purity detection
And (3) carrying out X-ray diffraction phase composition analysis on the sample obtained after high-temperature roasting, and comparing the sample with standard phase diffraction peak data of ilmenite. The results show that: the purity of the ferrotitanium sample prepared by the method is up to 96%.
Example 4
The preparation raw materials of the ilmenite of this embodiment include: the iron oxide, titanium dioxide, silicon dioxide and calcium oxide are prepared from the following raw materials in parts by mass:
the preparation method of the ilmenite comprises the following specific steps:
(1) Mixing the raw materials uniformly
Taking 20g of total mass of ferric oxide, titanium dioxide, silicon dioxide and calcium oxide according to the mass fraction, and fully and uniformly mixing the 20g of total mass in a mechanical mixer for 20min.
(2) Briquetting formation
The uniformly mixed raw materials are pressed into cylindrical samples with the height of 17mm and the diameter of 18mm in a tablet press under the pressure of 12Mpa.
(3) High temperature calcination
The pressed cylindrical test specimen was warmed from room temperature to 1100℃and incubated at this temperature for 30min.
(4) Purity detection
And (3) carrying out X-ray diffraction phase composition analysis on the sample obtained after high-temperature roasting, and comparing the sample with standard phase diffraction peak data of ilmenite. The results show that: the purity of the ferrotitanium sample prepared by the method is up to 94%.
Example 5
The preparation raw materials of the ilmenite of this embodiment include: the iron oxide, titanium dioxide, silicon dioxide and calcium oxide are prepared from the following raw materials in parts by mass:
the preparation method of the ilmenite comprises the following specific steps:
(1) Mixing the raw materials uniformly
Taking 15g of total mass of ferric oxide, titanium dioxide, silicon dioxide and calcium oxide according to the mass fraction, and fully and uniformly mixing the 15g of total mass in a mechanical mixer for 24min.
(2) Briquetting formation
The uniformly mixed raw materials are pressed into cylindrical samples with the height of 15mm and the diameter of 16mm in a tablet press under the pressure of 10 Mpa.
(3) High temperature calcination
The pressed cylindrical test specimen was warmed from room temperature to 1000℃and incubated at this temperature for 30min.
(4) Purity detection
And (3) carrying out X-ray diffraction phase composition analysis on the sample obtained after high-temperature roasting, and comparing the sample with standard phase diffraction peak data of ilmenite. The results show that: the purity of the ferrotitanium sample prepared by the method is up to 95%.
Comparative example 1
The preparation raw materials of this comparative example include: the iron oxide, titanium dioxide, silicon dioxide and calcium oxide are prepared from the following raw materials in parts by mass:
the preparation process of this comparative example is the same as in example 1.
Table 1 below shows the changes in the titanium garnet content, perovskite content and sinter index obtained after sintering in examples 1 to 5, based on comparative example 1. It can be seen from the combination of table 1 that the production of perovskite can be effectively inhibited by optimally controlling the content of each component, which is beneficial to the production of ilmenite, and the structural strength of the obtained sinter can be effectively improved.
TABLE 1 variation of the titanium garnet content, perovskite content and sinter index obtained in examples 1-5 relative to comparative example 1
Titanium garnet content | Perovskite content | Yield of sintered ore | Strength of sintered ore | |
Example 1 | +2% | -0.5% | +2% | +2% |
Example 2 | +1.8% | -0.2% | +1.5% | +1.6% |
Example 3 | +2.2% | -0.3% | +1.9% | +1.8% |
Example 4 | +1.6% | -0.1% | +1.6% | +1.4% |
Example 5 | +1.9% | -0.3% | +1.8% | +1.7% |
Claims (8)
2. the process for preparing ilmenite according to claim 1, characterized in that: specifically comprises the steps of raw material mixing, briquetting and roasting, wherein the roasting temperature is 1000-1250 ℃, and the heat preservation time is 20-30min.
3. The process for preparing ilmenite according to claim 2, characterized in that: when the raw materials are mixed, the raw materials of each component are placed in a mechanical mixer to be fully and uniformly mixed for 20-30min.
4. The process for preparing ilmenite according to claim 2, characterized in that: the evenly mixed raw materials are pressed into cylindrical samples with the height of 15-20mm and the diameter of 15-20mm in a tablet press.
5. The process for preparing ilmenite according to claim 4, wherein: the pressing pressure is 8-12Mpa.
6. The process for preparing ilmenite according to claim 2, characterized in that: and during roasting, the sample after being briquetted is directly heated from room temperature to the roasting temperature.
7. A method for inhibiting perovskite from generating in vanadium titano-magnetite sintering process is characterized by comprising the following steps: the vanadium titano-magnetite is used as a main raw material for batching, components of the mixture are regulated and controlled, and the mass parts of ferric oxide, titanium dioxide, silicon dioxide and calcium oxide in the mixture are controlled as follows:
8. the method for inhibiting perovskite formation during sintering of vanadium titano-magnetite according to claim 7, wherein the method comprises the steps of: the sintering temperature of the mixture is controlled to be 1000-1250 ℃ and the sintering time is controlled to be 20-30min.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2003027148A (en) * | 2001-07-12 | 2003-01-29 | Nippon Steel Corp | Method for manufacturing sintered ore |
CN101381809A (en) * | 2008-11-07 | 2009-03-11 | 攀枝花新钢钒股份有限公司 | Preparation method of vanadium titano-magnetite sinter |
CN106399673A (en) * | 2016-11-30 | 2017-02-15 | 重庆大学 | Method for improving compressive strength of vanadium titano-magnetite sintered ore |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2003027148A (en) * | 2001-07-12 | 2003-01-29 | Nippon Steel Corp | Method for manufacturing sintered ore |
CN101381809A (en) * | 2008-11-07 | 2009-03-11 | 攀枝花新钢钒股份有限公司 | Preparation method of vanadium titano-magnetite sinter |
CN106399673A (en) * | 2016-11-30 | 2017-02-15 | 重庆大学 | Method for improving compressive strength of vanadium titano-magnetite sintered ore |
Non-Patent Citations (1)
Title |
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陈贇: "二氧化钛在烧结过程中与铁酸钙反应的物相组成及反应规律研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》, pages 023 - 3 * |
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