CN112456550B - Method for preparing titanium slag with high acidolysis rate - Google Patents
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- CN112456550B CN112456550B CN202011241165.XA CN202011241165A CN112456550B CN 112456550 B CN112456550 B CN 112456550B CN 202011241165 A CN202011241165 A CN 202011241165A CN 112456550 B CN112456550 B CN 112456550B
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Abstract
The invention discloses a method for preparing titanium slag with high acidolysis rate, which comprises the following steps: (1) in the slag tapping process of titanium slag smelting, delivering molten titanium slag into a slag bucket; (2) adding a nucleating agent into the titanium slag, and uniformly mixing; (3) cooling the mixture in the step (2) under the hypergravity; (4) and (4) taking out the cooled mixture obtained in the step (3), cooling to room temperature, and removing a silicate phase through mechanical cutting to obtain the titanium slag with high acidolysis rate. The method of the invention introduces the added nucleating agent and the super-gravity field into the titanium slag melt, directionally enriches and separates out different phases in the titanium slag by controlling the cooling speed, and greatly improves the acidolysis rate of the titanium slag by removing the phase silicate phase which influences the acidolysis rate.
Description
Technical Field
The invention belongs to the field of titanium slag post-treatment and titanium white preparation, and particularly relates to a method for preparing titanium slag with high acidolysis rate, which is suitable for all titanium slag smelting fields and the titanium slag titanium white production field.
Background
The essence of the titanium slag smelted by the electric furnace is that ilmenite and solid reducing agent anthracite or petroleum coke are mixed and added into the electric furnace for reduction smelting, iron oxides in the ore are selectively reduced into metallic iron, titanium oxides are enriched in slag, and the slag iron is separated to obtain titanium slag and a byproduct metallic iron. The conventional production titanium slag is acid-soluble titanium slag for producing titanium dioxide by a sulfuric acid method, and the acidolysis rate of the titanium slag is greatly influenced by the phase composition, impurity components and the like of the titanium slag. The main phases of the acid-soluble titanium slag are a black titanium stone phase and a silicate phase, wherein 90-95% of the acid-soluble titanium slag is a black titanium stone solid solution and consists of a pseudobrookite phase (FeTi)2O5)a(MgTi2O5)b(Al2TiO5)c(MnTi2O5)d(V2TiO5)e(Ti3O5)fComposition, a + b + c + d + e + f ═ 1, the titanium oxide of the titanium nigrite solid solution is most soluble in sulfuric acid. 5-10% of silicate phase, which is silicate glass phase (Ca, Al, Mg, Fe, Ti) SiO3And (4) forming. Typical composition: SiO 2260％，Al2O318～20％，CaO9～10％，MgO1～4％，FeO2～4％，TiO 23 to 4%, and the silicate phase is hardly dissolved by sulfuric acid.
Therefore, in order to improve the acidolysis rate of the titanium slag, the insoluble phase silicate phase is mainly removed, and the soluble phase nigrolite phase is retained. As shown in the research on the influence of impurity oxides on the acidolysis rate, the increase of the content of MgO and FeO is beneficial to the acidolysis rate of the titanium slag, and the content of CaO and SiO is beneficial to the acidolysis rate of the titanium slag2And Al2O3The acid solubility of the titanium slag is reduced along with the increase of the content. In the above, it can be seen from the study of the occurrence of impurities that the biotite phase mainly comprises elements such as Ti, Fe, and Mg, and the silicate glass phase mainly comprises elements such as Ca, Al, and Si. Therefore, the contents of MgO and FeO which are favorable for the acidolysis rate mainly exist in the titanium black phase, and most of impurity elements CaO and SiO which are not favorable for the acidolysis rate2And Al2O3Present in the silicate phase.
Therefore, the content of impurity elements in the silicate phase is also reduced to increase the acid hydrolysis rate. And the silicate glass phase is dispersed and mixed in the titanium black solid solution, has fine embedded particle size and is mostly wrapped. On the premise of ensuring the particle size and the titanium yield of the titanium slag, the silicate phase and the titanium black phase are difficult to be effectively separated by the conventional fine grinding and magnetic separation technology.
Based on the above, there is a need for developing a novel phase separation method which can effectively ensure the particle size and titanium yield of titanium slag and effectively remove silicate phase.
Disclosure of Invention
In view of the above, it is necessary to adopt the following technical solutions:
the invention provides a method for preparing titanium slag with high acidolysis rate, which comprises the following steps:
(1) in the slag tapping process of titanium slag smelting, delivering molten titanium slag into a slag bucket;
(2) adding a nucleating agent into the titanium slag, and uniformly mixing;
(3) cooling the mixture in the step (2) under the hypergravity;
(4) and (4) taking out the cooled mixture obtained in the step (3), cooling to room temperature, and removing a silicate phase through mechanical cutting to obtain the titanium slag with high acidolysis rate.
Further, the slag discharging temperature of the titanium slag in the step (1) is 1680-1750 ℃.
Further, the nucleating agent is CaO and Al2O3、SiO2One or more of (a).
Furthermore, the addition amount of the nucleating agent accounts for 2 to 5 percent of the weight of the titanium slag.
Further, the cooling rate in the step (3) is 10-25 k/min. Adding additive and controlling cooling speed to make the silicate phase to be separated selectively precipitate and grow.
Further, the gravity coefficient of the supergravity in the step (3) is 600-850. The method is characterized in that the relative movement distance between the two phases is increased in a high gravity field by utilizing different specific gravities of the black titanium phase and the silicate phase in the titanium slag, so that the two phases are distributed in different areas in a centrifugal field.
Further, cooling the mixture in the step (2) to 1000-1100 ℃ under the hypergravity, and stopping cooling.
Further, in the cooling process in the step (3), one of tap water, frozen saline and liquid nitrogen is adopted to cool the slag barrel.
Further, after the hypergravity cooling in the step (3), the silicate phase can present a particle size gradient distribution along the direction of the hypergravity, so that the silicate phase is enriched on one side of the mixture, and the silicate phase can be removed through mechanical cutting.
The invention also provides a method for producing titanium dioxide by a sulfuric acid method, which takes the titanium slag with high acidolysis rate prepared by the method as a raw material. As for the method for producing titanium dioxide by the sulfuric acid process, a method commonly used in the prior art, such as the method disclosed in CN 102277489A, is adopted, and details are not described herein.
The invention has the following beneficial technical effects:
the invention discloses a method for rapidly improving the acidolysis rate of titanium slag. In particular to a method for adding a nucleating agent and introducing a super-gravity field into a titanium slag melt, directionally enriching and separating out different phases in the titanium slag by controlling the cooling speed, and greatly improving the acidolysis rate of the titanium slag by removing a phase silicate phase which influences the acidolysis rate.
The invention selectively separates and grows silicate phases to be separated by adding additives and controlling the cooling speed, increases the relative movement distance between two phases in a supergravity field by utilizing different specific gravities of the black titanium phase and the silicate phase in the titanium slag, so that the two phases are distributed in different areas in a centrifugal field, and then separates and removes the silicate phase in slag after physical cutting, thereby improving the acidolysis rate of the titanium slag and providing a high-quality raw material for titanium white production by a sulfuric acid method.
Compared with the existing fine grinding and magnetic separation technology, the titanium slag phase separation technology provided by the invention is simple in process and environment-friendly.
The separation technology has higher Ti yield, and the acidolysis rate of the titanium slag is improved to more than 95 percent from about 88 percent in the prior art. Wherein the prior acidolysis rate of about 88 percent is the acidolysis data of acid-soluble slag produced by adopting the prior cooling system of a titanium slag plant.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other embodiments can be obtained according to the drawings without creative efforts;
FIG. 1 is a schematic cross-sectional view of a slag ladle of an embodiment of the invention;
FIG. 2 is a flow chart of the method for preparing titanium slag with high acidolysis rate according to the embodiment of the invention.
Description of the reference numerals
1, a slag bucket; 2, an outer barrel; 3, an inner barrel; 4 a rotating shaft; 5, a top cover; 6, hanging rings; 7 cooling liquid inlet; 8, a cooling liquid pipeline outlet;
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following embodiments of the present invention are described in further detail with reference to the accompanying drawings.
As shown in fig. 1, the slag ladle 1 used in this embodiment includes an outer ladle 2 and an inner ladle 3 disposed inside the outer ladle 2; a rotating shaft 4 is arranged at the center of the bottom of the outer barrel 2; after the inner tub 3 is placed on the outer tub 2, the rotation shaft 4 passes through the inner tub 3 to connect the inner tub 3 and the outer tub 2 so that the inner tub 3 can rotate with respect to the outer tub 2; a top cover 5 is arranged above the inner barrel 3 to seal the inner barrel 3; the inner barrel 3 can move up and down along the direction of the rotating shaft 4 to realize the taking and placing functions.
The hanging rings 6 are symmetrically arranged on two sides of the barrel body of the inner barrel 3, so that the lifting is convenient; a motor (not shown) controls the rotation rate of the rotating shaft 4, and the gravity coefficient of the hot slag in the inner barrel 3 is controlled by adjusting the frequency of the motor to control the rotating shaft 4. The inner lining of the inner barrel 3, the surface of the rotating shaft 4 and the inner surface of the top cover 5 are coated with release agents.
An annular cooling liquid pipeline is arranged on the wall of the outer barrel 2 surrounding the outer barrel 2, and the cooling speed of the slag in the inner barrel 3 is controlled by adjusting the flow rate of the cooling medium. The cooling liquid pipeline adopts a form of up-in and down-out, namely, the upper part of the wall of the outer barrel 2 is provided with a cooling liquid pipeline inlet 7, and the lower part of the wall of the outer barrel 2 is provided with a cooling liquid pipeline outlet 8.
The method for preparing the titanium slag with high acidolysis rate as shown in FIG. 2 comprises the following steps:
(1) in the slag tapping process of titanium slag smelting, delivering molten titanium slag into a slag bucket 1;
(2) after the molten titanium slag enters the slag bucket 1, adding a nucleating agent into the titanium slag, and uniformly mixing;
(3) cooling the mixture in the step (2) under the hypergravity condition to a specific temperature;
(4) and (4) taking out the cooled mixture obtained in the step (3), cooling to room temperature (normally, water cooling the titanium slag to room temperature), and separating a titanium black phase and a silicate phase in the slag through mechanical cutting to obtain the titanium slag with high acidolysis rate.
Preferably, the slag discharging temperature of the titanium slag in the step (1) is 1680-1750 ℃.
Preferably, the nucleating agent is CaO, Al2O3、SiO2One or more of (a).
Preferably, the addition amount of the nucleating agent accounts for 2 to 5 percent of the weight of the titanium slag.
Preferably, in order to ensure the precipitation and growth of crystals in the silicate phase, the cooling rate in step (3) is preferably 10 to 25 k/min. Adding additive and controlling cooling speed to make the silicate phase to be separated selectively precipitate and grow.
Preferably, the gravity coefficient of the supergravity in the step (3) is 600-850, and correspondingly, the rotation speed of the inner cylinder is about 1000-1800 r/min. The method is characterized in that the relative movement distance between the two phases is increased in a high gravity field by utilizing different specific gravities of the black titanium phase and the silicate phase in the titanium slag, so that the two phases are distributed in different areas in a centrifugal field.
Preferably, the mixture in the step (2) is cooled to 1000-1100 ℃ under the super-gravity, the cooling under the super-gravity is stopped, and then the inner barrel 3 is taken out and cooled to the room temperature by water.
Preferably, the cooling process in the step (3) adopts one of tap water, frozen saline and liquid nitrogen to cool the slag ladle 1.
Preferably, after said hypergravity treatment in step (3), the silicate phase will exhibit a particle size gradient distribution along the direction of the hypergravity (the direction of the centrifugal force). In the rotating process of the rotating shaft, the silicate phase is fully contacted with the nucleating agent, and particles in the silicate phase are precipitated and grown up due to the control of the nucleating agent and the cooling speed, so that large-particle silicate phase grains can be enriched at the bottom of the sample in the process of cooling the sample to room temperature by water, and the silicate phase can be removed by mechanical cutting.
Example 1
The slag temperature of the titanium slag is 1718 ℃, the hot slag is put into a slag bucket, and Al accounting for 1 percent of the weight of the titanium slag is added into the slag bucket2O3And 3% of SiO2And (3) covering the inner barrel, sealing the inner barrel, introducing cooling water into the outer slag barrel to cool the titanium slag at a cooling rate of 20k/min, controlling the gravity coefficient to be 750, cooling the titanium slag to 1050 ℃ under the condition of supergravity, taking out the slag barrel, placing the slag barrel in a water-cooling pool to cool to room temperature, and cutting to remove a silicate phase at the bottom of the titanium slag. The upper titanium slag is crushed to-200 meshes and then placed in sulfuric acid for acidolysis, and the acidolysis rate of the titanium slag is 95.44%.
Example 2
The tapping temperature of the titanium slag is 1742 ℃, the hot slag is put into a slag bucket, and CaO accounting for 1 percent of the weight of the titanium slag and SiO accounting for 3 percent of the weight of the titanium slag are added into the slag bucket2And (3) covering the inner barrel, sealing the inner barrel, introducing cooling water into the outer slag barrel, cooling the titanium slag at a cooling rate of 25k/min, controlling the gravity coefficient to be 800, cooling the titanium slag to 1000 ℃ under the condition of supergravity, taking out the slag barrel, placing the slag barrel in a water-cooling pool, cooling to room temperature, and cutting to remove a silicate phase at the bottom of the titanium slag. Crushing the upper titanium slag to-200 meshes, and then placing the crushed upper titanium slag into sulfuric acid for acidolysis to obtain 95.71% of titanium slag acidolysis rate.
Example 3
The tapping temperature of the titanium slag is 1742 ℃, the hot slag is put into a slag bucket, and SiO 3 percent of the weight of the titanium slag is added into the slag bucket2And (3) powder is obtained, the inner barrel is sealed by covering, the titanium slag is cooled at a cooling rate of 10k/min by introducing cooling water into the outer slag barrel, the gravity coefficient is controlled to be 800, the titanium slag is cooled to 1000 ℃ under the condition of supergravity, the slag barrel is taken out, the slag barrel is placed in a water cooling tank to be cooled to room temperature, and a silicate phase at the bottom of the titanium slag is removed by cutting. Crushing the upper titanium slag to-200 meshes, and then placing the crushed upper titanium slag into sulfuric acid for acidolysis to obtain 97.26% of titanium slag acidolysis rate.
The foregoing is an exemplary embodiment of the present disclosure, but it should be noted that various changes and modifications could be made herein without departing from the scope of the present disclosure as defined by the appended claims. Although elements of the disclosed embodiments of the invention may be described or claimed in the singular, the plural is contemplated unless limitation to the singular is explicitly stated.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, of embodiments of the invention is limited to these examples; within the idea of an embodiment of the invention, also technical features in the above embodiment or in different embodiments may be combined and there are many other variations of the different aspects of the embodiments of the invention as described above, which are not provided in detail for the sake of brevity. Therefore, any omissions, modifications, substitutions, improvements, and the like that may be made without departing from the spirit and principles of the embodiments of the present invention are intended to be included within the scope of the embodiments of the present invention.
Claims (6)
1. The method for preparing the titanium slag with high acidolysis rate is characterized by comprising the following steps:
(1) in the slag tapping process of titanium slag smelting, delivering molten titanium slag into a slag bucket;
(2) adding a nucleating agent into the titanium slag, and uniformly mixing; the addition amount of the nucleating agent accounts for 2 to 5 percent of the weight of the titanium slag; the nucleating agent is CaO and Al2O3、SiO2One or more of;
(3) cooling the mixture in the step (2) under the condition of supergravity, wherein the cooling rate is 10-25 k/min; after the hypergravity cooling, the silicate phase presents the particle size gradient distribution along the hypergravity direction so as to realize that the silicate phase is enriched on one side of the mixture;
(4) and (4) taking out the cooled mixture obtained in the step (3), cooling to room temperature, and removing a silicate phase through mechanical cutting to obtain the titanium slag with high acidolysis rate.
2. The method for preparing the titanium slag with high acidolysis rate as claimed in claim 1, wherein the slag tapping temperature of the titanium slag in the step (1) is 1680-1750 ℃.
3. The method for preparing titanium slag with high acidolysis rate according to claim 1, wherein the gravity coefficient of the hypergravity in the step (3) is 600-850.
4. The method for preparing titanium slag with high acidolysis rate according to claim 1, wherein the mixture in step (2) is cooled to 1000-1100 ℃ under the supergravity, and the cooling is stopped.
5. The method for preparing titanium slag with high acidolysis rate as claimed in claim 1, wherein the cooling process in step (3) adopts one of tap water, frozen saline water and liquid nitrogen to cool the slag ladle.
6. A method for producing titanium dioxide by a sulfuric acid process, which is characterized in that the method takes the titanium slag with high acidolysis rate, which is prepared by the method of any one of claims 1 to 5, as a raw material.
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Effective date of registration: 20230918 Address after: 617000 Taoyuan street, East District, Panzhihua, Sichuan Province, No. 90 Patentee after: PANGANG GROUP PANZHIHUA IRON & STEEL RESEARCH INSTITUTE Co.,Ltd. Patentee after: Chengdu advanced metal material industry technology Research Institute Co.,Ltd. Address before: 617000 Taoyuan street, East District, Panzhihua, Sichuan Province, No. 90 Patentee before: PANGANG GROUP PANZHIHUA IRON & STEEL RESEARCH INSTITUTE Co.,Ltd. |