CN112961993B - Method for extracting titanium from vanadium titano-magnetite smelting slag - Google Patents
Method for extracting titanium from vanadium titano-magnetite smelting slag Download PDFInfo
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- CN112961993B CN112961993B CN202110137012.9A CN202110137012A CN112961993B CN 112961993 B CN112961993 B CN 112961993B CN 202110137012 A CN202110137012 A CN 202110137012A CN 112961993 B CN112961993 B CN 112961993B
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- smelting slag
- vanadium titano
- titanium
- magnetite smelting
- magnetite
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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
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1204—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent
- C22B34/1209—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent by dry processes, e.g. with selective chlorination of iron or with formation of a titanium bearing slag
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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
Abstract
The invention discloses a method for extracting titanium from vanadium titano-magnetite smelting slag, which comprises the following steps: pretreating vanadium titano-magnetite smelting slag;adding B into pretreated vanadium titano-magnetite smelting slag2O3Or solid boric acid to obtain a first material; roasting the first material at low temperature in a reducing atmosphere to obtain a second material; and (3) roasting the second material at high temperature in a reducing atmosphere, preserving heat for the first time, cooling to 200-400 ℃ at the speed of 2-10 ℃/min, preserving heat for the second time, and naturally cooling to room temperature to obtain the titanium schorl phase titanium ore. The method can realize the enrichment of titanium in the vanadium titano-magnetite smelting slag and improve the enrichment degree and grade of the titanium.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to a method for extracting titanium from vanadium titano-magnetite smelting slag.
Background
Vanadium titano-magnetite is a kind of multi-element paragenic ore, and its composition varies with the producing area. Mainly used as raw materials for extracting iron, vanadium and titanium. The mined ore is subjected to mineral separation to obtain vanadium-containing iron ore concentrate which is used as a raw material for smelting steel. The tailings from iron separation are used to recover ilmenite concentrates (referred to simply as titanium concentrates) for use as a feed for extracting titanium products. The ferrovanadium magnetite has abundant reserves in the world, the reserves of China are listed as the top festuca, and the reserves of the Panxi area in Sichuan reach billions of tons, which account for more than 80 percent of the reserves in the country. But the titanium sand ore resources are less, the distribution is more dispersed, and a large titanium sand ore deposit is not found so far. In the smelting process of the vanadium titano-magnetite, a large amount of vanadium titano-magnetite smelting slag is generated, except a small part of vanadium titano-magnetite smelting slag is used for building materials, most of the vanadium titano-magnetite smelting slag is accumulated in a slag field, the vanadium titano-magnetite smelting slag mainly comprises oxides of Fe, Ti, Si, Mg, Al, Ca, V and S, and the large amount of vanadium titano-magnetite smelting slag is accumulated into a mountain, so that the high-value titanium resource is wasted, the environment is polluted, and if titanium can be recovered from the vanadium titano-magnetite smelting slag, the vanadium titano-magnetite smelting slag has great economic value and social benefit.
Disclosure of Invention
The invention aims to provide a method for extracting titanium from vanadium titano-magnetite smelting slag, which improves the grade of the titanium in the recovered titanium concentrate.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a method for extracting titanium from vanadium titano-magnetite smelting slag, which comprises the following steps:
(1) pretreating vanadium titano-magnetite smelting slag;
(2) adding B into pretreated vanadium titano-magnetite smelting slag2O3Or solid boric acid to obtain a first material;
(3) roasting the first material at low temperature in a reducing atmosphere to obtain a second material; the reducing atmosphere comprises CO atmosphere or H2An atmosphere;
(4) and roasting the second material at high temperature in a reducing atmosphere, preserving heat, cooling to 200-400 ℃ at the speed of 2-10 ℃/min, preserving heat, and naturally cooling to room temperature to obtain the titanite rich in the black titanite phase.
Preferably, the pretreatment process in the step (1) is to add chloride auxiliary agent into the vanadium titano-magnetite smelting slag, mix, ball mill, and ball mill until the material with about 90 meshes accounts for more than 90 wt%.
Preferably, the addition amount of the chloride salt auxiliary agent in the step (1) is 0.3-0.5 wt% of the vanadium titano-magnetite smelting slag.
Preferably, the chloride salt adjuvant of step (1) comprises ammonium chloride or aluminum trichloride.
Preferably, said step (2) B2O3Or the addition amount of the solid boric acid is 0.01-0.05 wt% of the vanadium titano-magnetite smelting slag.
Preferably, the low-temperature roasting in the step (3) is 200-400 ℃.
Preferably, the high-temperature roasting in the step (4) is 800-1000 ℃, the first heat preservation is performed for 20-30min, and the second heat preservation is performed for 60-120 min.
The invention discloses the following technical effects:
firstly, preprocessing vanadium titano-magnetite smelting slag, adding a chloride salt auxiliary agent in the ball milling process, ball milling until the material with about 90 meshes accounts for more than 90wt%, and adding B into the preprocessed vanadium titano-magnetite smelting slag2O3Or solid boric acid additive to obtain a first material, then roasting at low temperature in a reducing atmosphere, then roasting at high temperature in a reducing atmosphere, and forming a black titanium ore phase through the process to realize vanadium-titanium magnetite metallurgyAnd (3) enriching titanium in the smelting slag, wherein the enrichment degree of the titanium is over 50 percent, and the grade of the titanium in the black titanium stone phase is over 90 percent. The method can separate and utilize the titanium-rich phase in large quantity, has simple process, less added additive amount, higher titanium-containing grade of the obtained titanium-rich black titanite, convenient separation and utilization and larger social and economic benefits.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The method for calculating the titanium enrichment degree comprises the following steps:
example 1
A method for extracting titanium from vanadium titano-magnetite smelting slag specifically comprises the following steps:
(1) carrying out pretreatment on vanadium titano-magnetite smelting slag: adding 0.3wt% of ammonium chloride into vanadium titano-magnetite smelting slag, mixing, ball-milling until the proportion of materials with about 90 meshes is more than 90 wt%;
(2) adding 0.01wt% of B into the pretreated vanadium titano-magnetite smelting slag2O3Obtaining a first material;
(3) at H2Roasting the first material at the low temperature of 200 ℃ under the atmosphere to obtain a second material;
(4) and roasting the second material at the high temperature of 800 ℃ in a reducing atmosphere, preserving heat for 20min, cooling to 400 ℃ at the speed of 5 ℃/min, preserving heat for 80min, and naturally cooling to room temperature to obtain the titanite rich in the black titanium ore phase, wherein the enrichment degree of titanium is 52%, and the grade of titanium is 90%.
Example 2
A method for extracting titanium from vanadium titano-magnetite smelting slag specifically comprises the following steps:
(1) carrying out pretreatment on vanadium titano-magnetite smelting slag: adding 0.4wt% of aluminum trichloride into the vanadium titano-magnetite smelting slag, mixing, and performing ball milling until the material with about 90 meshes accounts for more than 90 wt%;
(2) adding 0.01wt% of B into the pretreated vanadium titano-magnetite smelting slag2O3Obtaining a first material;
(3) roasting the first material at a low temperature of 300 ℃ in a CO atmosphere to obtain a second material;
(4) and roasting the second material at the high temperature of 800 ℃ in a reducing atmosphere, preserving heat for 30min, cooling to 400 ℃ at the speed of 5 ℃/min, preserving heat for 60min, and naturally cooling to room temperature to obtain the titanite rich in a black titanium ore phase, wherein the enrichment degree of titanium is 60%, and the grade of titanium is 93%.
Example 3
A method for extracting titanium from vanadium titano-magnetite smelting slag specifically comprises the following steps:
(1) carrying out pretreatment on vanadium titano-magnetite smelting slag: adding 0.5wt% of aluminum trichloride into the vanadium titano-magnetite smelting slag, mixing, and performing ball milling until the material with about 90 meshes accounts for more than 90 wt%;
(2) adding 0.03wt% of solid boric acid into the pretreated vanadium titano-magnetite smelting slag to obtain a first material;
(3) at H2Roasting the first material at the low temperature of 200 ℃ under the atmosphere to obtain a second material;
(4) and roasting the second material at the high temperature of 1000 ℃ in a reducing atmosphere, preserving heat for 20min, cooling to 400 ℃ at the speed of 8 ℃/min, preserving heat for 80min, and naturally cooling to room temperature to obtain the titanite rich in a black titanium ore phase, wherein the enrichment degree of titanium is 65%, and the grade of titanium is 95%.
Example 4
A method for extracting titanium from vanadium titano-magnetite smelting slag specifically comprises the following steps:
(1) carrying out pretreatment on vanadium titano-magnetite smelting slag: adding 0.5wt% of ammonium chloride into vanadium titano-magnetite smelting slag, mixing, ball-milling until the proportion of materials with about 90 meshes is more than 90 wt%;
(2) adding 0.05wt% of B into the pretreated vanadium titano-magnetite smelting slag2O3Obtaining a first material;
(3) at H2Roasting the first material at a low temperature of 300 ℃ under the atmosphere to obtain a second material;
(4) and roasting the second material at the high temperature of 800 ℃ in a reducing atmosphere, preserving heat for 20min, cooling to 400 ℃ at the speed of 5 ℃/min, preserving heat for 120min, and naturally cooling to room temperature to obtain the titanite rich in a black titanium ore phase, wherein the enrichment degree of titanium is 55%, and the grade of titanium is 91%.
Example 5
A method for extracting titanium from vanadium titano-magnetite smelting slag specifically comprises the following steps:
(1) carrying out pretreatment on vanadium titano-magnetite smelting slag: adding 0.3wt% of ammonium chloride into vanadium titano-magnetite smelting slag, mixing, ball-milling until the proportion of materials with about 90 meshes is more than 90 wt%;
(2) adding 0.01wt% of B into the pretreated vanadium titano-magnetite smelting slag2O3Obtaining a first material;
(3) at H2Roasting the first material at a low temperature of 400 ℃ in an atmosphere to obtain a second material;
(4) and roasting the second material at the high temperature of 900 ℃ in a reducing atmosphere, keeping the temperature for 25min, cooling to 200 ℃ at the speed of 2 ℃/min, keeping the temperature for 100min, and naturally cooling to room temperature to obtain the titanite rich in the black titanium ore phase, wherein the enrichment degree of titanium is 55%, and the grade of titanium is 90%.
Comparative example 1
The difference from the example 3 is that solid boric acid is directly added into the vanadium titano-magnetite smelting slag without pretreatment, the enrichment degree of titanium is 22 percent, and the grade of titanium is 88 percent.
Comparative example 2
The difference from example 3 is only that the firing process is as follows: after addition of solid boric acid, in H2Under the atmosphere, melting the first material at 1300 ℃ for 20min, cooling to 1200 ℃ at a cooling rate of 8 ℃/min, then preserving heat for 80min, directly throwing the first material into ice water for quenching after heat preservation, wherein the enrichment degree of titanium is 25%, and the grade of titanium is 90%.
Comparative example 3
The only difference from example 3 is that step (3) is O2The method is carried out in the atmosphere, the enrichment degree of titanium is 15%, and the grade of titanium is 85%.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (1)
1. A method for extracting titanium from vanadium titano-magnetite smelting slag is characterized by comprising the following steps:
(1) pretreating vanadium titano-magnetite smelting slag, wherein the pretreatment process comprises the steps of adding a chloride auxiliary agent into the vanadium titano-magnetite smelting slag, mixing, and carrying out ball milling, wherein the adding amount of the chloride auxiliary agent is 0.3-0.5 wt% of the vanadium titano-magnetite smelting slag, and the chloride auxiliary agent is ammonium chloride or aluminum trichloride;
(2) adding B into pretreated vanadium titano-magnetite smelting slag2O3Or solid boric acid to obtain a first material, B2O3Or the addition amount of the solid boric acid is 0.01-0.05 wt% of the vanadium titano-magnetite smelting slag;
(3) roasting the first material at low temperature of 200-400 ℃ in a reducing atmosphere to obtain a second material;
(4) and (3) roasting the second material at high temperature in a reducing atmosphere, preserving heat, cooling to 200-400 ℃ at the speed of 2-10 ℃/min, preserving heat, roasting at high temperature of 800-1000 ℃, preserving heat for 20-30min for the first time, preserving heat for 60-120min for the second time, and naturally cooling to room temperature to obtain the titanium ore rich in the biotite phase.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103468962B (en) * | 2013-08-21 | 2015-02-11 | 北京科技大学 | Titanium beneficiation method from titaniferous blast furnace slag |
| CN106048256B (en) * | 2016-06-30 | 2018-01-05 | 重庆大学 | Method for removing calcium and magnesium impurities in titanium slag by using modified additive |
| CN109252053B (en) * | 2018-11-14 | 2020-06-23 | 西南科技大学 | Method for extracting titanium, carbon and chlorine components from titanium-containing slag by virtue of sectional roasting separation |
| CN109321759B (en) * | 2018-11-14 | 2020-04-10 | 西南科技大学 | Method for extracting titanium, iron, aluminum and magnesium components in high-titanium slag by virtue of sectional roasting |
| CN109439918B (en) * | 2018-11-14 | 2020-08-21 | 西南科技大学 | System for extracting titanium, iron, aluminum and magnesium components in high-titanium slag through fractional roasting |
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