Oxidation method of high titanium slag

Abstract

The invention relates to an oxidation method of high titanium slag, and belongs to the technical field of mineral resource processing and utilization and inorganic functional material preparation processes. The method comprises the following steps: obtaining to-be-oxidized high titanium slag; the high titanium slag is subjected to heating oxidation treatment, the atmosphere of the heating oxidation treatment comprises H2O, oxidation is completed, and a product is obtained; h2O is introduced into the atmosphere of the heating oxidation treatment, and the H2O can play a role in catalyzing the heating oxidation treatment of the high titanium slag, so that the oxidation treatment efficiency of the high titanium slag is improved. And the phase of the product finally prepared by the method is consistent with the phase obtained by treatment only in the oxygen atmosphere.

Description

Technical Field

[0001] The present application relates to the technical field of mineral resource processing and utilization and inorganic functional material preparation technology, and in particular to a method for oxidizing high-titanium slag. Background Art

[0002] High-titanium slag is a product obtained by carbon-thermal reduction of ilmenite, and is an important raw material for the production of titanium dioxide and sponge titanium. With the development of the titanium industry, natural rutile resources with high titanium grades are becoming less and less, and ilmenite has become the main available resource for the titanium industry. Through carbon-thermal reduction of ilmenite, the high-valent iron in ilmenite is reduced, and the high-valent titanium is simultaneously reduced to low-valent titanium and enriched in high-titanium slag. The grade of TiO2 in high-titanium slag is quite high, and the composition is complex, mainly in the form of black titanium and anatase. Among them, FeO and Ti2O3 in the slag dissolve each other to form a solid solution with M3O5 as the main phase, which is usually called "iron brookite (Fe2TiO5)"; Ti2O3 is easily oxidized in subsequent processing (after ilmenite (FeTiO3) is refined from the furnace to slag). In view of the many adverse effects of low-valent titanium on subsequent processes, low-valent titanium in high-titanium slag must be oxidized to high-valent titanium.

[0003] Some people have proposed to convert low-valent titanium in high-titanium slag into rutile TiO2 by oxidative roasting at 1000℃, and remove impurities such as S, P, and C at the same time. Oxidative roasting is currently a major step in the treatment of high-titanium slag, which can effectively convert low-valent titanium into high-valent titanium. However, its treatment efficiency still needs to be improved. Summary of the invention

[0004] The present application provides a method for oxidizing high-titanium slag, which can improve the oxidation treatment efficiency of high-titanium slag.

[0005] The present application provides a method for oxidizing high-titanium slag, the method comprising:

[0006] Obtaining high-titanium slag to be oxidized;

[0007] The high-titanium slag is subjected to a heating oxidation treatment, wherein the atmosphere of the heating oxidation treatment includes H2O, and oxidation is completed to obtain a product.

[0008] As an optional implementation, in the atmosphere of the heating oxidation treatment, the volume proportion of H2O is 12% to 20%.

[0009] As an optional implementation, the atmosphere of the heating oxidation treatment is an oxygen-containing atmosphere.

[0010] As an optional implementation, in the atmosphere of the heating oxidation treatment, the volume proportion of O2 is 12% to 20%.

[0011] As an optional embodiment, the atmosphere composition of the heating oxidation treatment includes, by volume fraction, 12% to 20% O2 and 12% to 20% H2O, with the remainder being inert gas and / or nitrogen.

[0012] As an optional implementation, the inert gas includes argon.

[0013] As an optional implementation, the particle size of the high titanium slag is 425 μm to 600 μm.

[0014] As an optional implementation manner, the temperature of the heating oxidation treatment is 700°C to 900°C.

[0015] As an optional implementation manner, the heating oxidation treatment time is 1 hour to 2 hours.

[0016] As an optional embodiment, the flow rate of the heated oxidation atmosphere is not less than 2 dm 3 / min.

[0017] The above technical solution provided by the embodiment of the present application has the following advantages compared with the prior art:

[0018] The method provided in the embodiment of the present application, by introducing H2O into the atmosphere of the heating oxidation treatment, H2O can play a catalytic effect on the heating oxidation treatment of high-titanium slag, thereby improving the oxidation treatment efficiency of high-titanium slag. And the product phase finally obtained by this method is consistent with the phase obtained by treating only in an oxygen atmosphere. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present application and, together with the description, serve to explain the principles of the present application.

[0020] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative labor.

[0021] Figure 1 A flowchart of the method provided in the embodiment of the present application. DETAILED DESCRIPTION

[0022] In order to make the purpose, technical solution and advantages of the embodiments of the present application clearer, the technical solution in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of this application.

[0023] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in this application can be purchased from the market or prepared by existing methods.

[0024] Figure 1 A flow chart of the method provided in the embodiment of the present application is as follows: Figure 1 As shown, the embodiment of the present application provides a method for oxidizing high-titanium slag, the method comprising:

[0025] S1. Obtaining high titanium slag to be oxidized;

[0026] In some embodiments, the particle size of the high titanium slag is 425 μm to 600 μm. For example, the particle size of the high titanium slag can be 425 μm, 430 μm, 435 μm, 440 μm, 445 μm, 450 μm, 455 μm, 460 μm, 465 μm, 470 μm, 475 μm, 480 μm, 485 μm, 490 μm, 495 μm, 500 μm, 505 μm, 510 μm, 520 μm, 530 μm, 540 μm, 550 μm, 560 μm, 570 μm, 580 μm, 590 μm or 600 μm, etc., and it can also be any value within the range of 425 μm to 600 μm.

[0027] Specifically, in this embodiment, the raw material high titanium slag is crushed into high titanium slag powder with a particle size of 425 to 600 μm to obtain high titanium slag to be oxidized.

[0028] S2. The high-titanium slag is subjected to a heating oxidation treatment, wherein the atmosphere of the heating oxidation treatment includes H2O, and the oxidation is completed to obtain a product.

[0029] Specifically, in this embodiment, a 30g high-titanium slag sample to be oxidized is placed in a silicon container and heated and oxidized on a fluidized bed in a vertical tubular furnace. After the sample is placed in the reactor, it is protected by liquefied inert gas and the furnace temperature is kept constant. Then, an oxidizing mixed gas is introduced, and the flow rate of the mixed gas at room temperature is not less than 2dm 3 / min. The flow rate of the mixed gas is controlled by a flow controller; then the treated sample is protected by an inert gas until it is cooled enough to be weighed.

[0030] In some embodiments, in the atmosphere of the heating oxidation treatment, the volume proportion of H2O is 12% to 20%.

[0031] Exemplarily, the volume percentage of H2O in the atmosphere of the heated oxidation treatment can be 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19% or 20%, etc., and it can also be any value in the range of 12% to 20%.

[0032] In some embodiments, the atmosphere of the heating and oxidation treatment is an oxygen-containing atmosphere. Further, in the atmosphere of the heating and oxidation treatment, the volume proportion of O2 is 12% to 20%.

[0033] Exemplarily, the volume percentage of O2 in the atmosphere of the heated oxidation treatment can be 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19% or 20%, etc., and it can also be any value within the range of 12% to 20%.

[0034] In some embodiments, the atmosphere composition of the heating oxidation treatment includes, by volume fraction, 12% to 20% O2 and 12% to 20% H2O, with the remainder being inert gas and / or nitrogen. Further, the inert gas includes argon. It will be appreciated by those skilled in the art that, in other embodiments, the inert gas may also be selected from helium, neon, etc.

[0035] In some embodiments, the temperature of the heating oxidation treatment is 700° C. to 900° C. Exemplarily, the temperature of the heating oxidation treatment can be 700° C., 710° C., 720° C., 730° C., 740° C., 750° C., 760° C., 770° C., 780° C., 790° C., 800° C., 810° C., 820° C., 830° C., 840° C., 850° C., 860° C., 870° C., 880° C., 890° C. or 900° C., etc., and can also be any value within the range of 700° C. to 900° C.

[0036] In some embodiments, the heating oxidation treatment time is 1 h to 2 h. Exemplarily, the heating oxidation treatment time can be 1 h, 1.1 h, 1.2 h, 1.3 h, 1.4 h, 1.5 h, 1.6 h, 1.7 h, 1.8 h, 1.9 h or 2 h, etc., and it can also be any value within the range of 1 h to 2 h.

[0037] The method introduces H2O into the atmosphere of the heating oxidation treatment, and H2O can play a catalytic effect on the heating oxidation treatment of high-titanium slag, thereby improving the oxidation treatment efficiency of high-titanium slag. In addition, the product phase obtained by the method is consistent with the phase obtained by treating only in an oxygen atmosphere.

[0038] The present application will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are intended only to illustrate the present application and are not intended to limit the scope of the present application. The experimental methods for which specific conditions are not specified in the following examples are usually measured according to national standards. If there is no corresponding national standard, then the conditions recommended by the manufacturer are followed.

[0039] Example 1

[0040] A method for oxidizing high-titanium slag, the method comprising:

[0041] First, weigh 30g of high titanium slag, the chemical composition of the slag is: ∑TiO2: 92.65%, S: 0.016%, P: 0.014%, C: 0.049% and ∑Fe: 5.26%. Grind the raw materials to a particle size of 425-600μm, then put the raw materials into a fluidized bed of a vertical tubular furnace, introduce liquefied protective gas Ar, keep the furnace temperature constant for 12 minutes, then replace the gas with an oxidizing mixed gas, the composition is 12% O2 and 12% H2O Ar, the mixed gas flow is controlled by a flow controller, the minimum is 2dm 3 / min. Then heat the material to 800℃ and keep the temperature constant for 1h. Protect the sample with inert gas until it cools down enough to be weighed.

[0042] Example 2

[0043] A method for oxidizing high-titanium slag, the method comprising:

[0044] First, weigh 30g of high titanium slag, the chemical composition of the slag is: ∑TiO2: 92.65%, S: 0.016%, P: 0.014%, C: 0.049% and ∑Fe: 5.26%. Grind the raw materials to a particle size of 425-600μm, then put the raw materials into a fluidized bed of a vertical tubular furnace, introduce liquefied protective gas Ar, keep the furnace temperature constant for 15 minutes, then replace the gas with an oxidizing mixed gas, the composition is 15% O2 and 15% H2O Ar, the mixed gas flow is controlled by a flow controller, the minimum is 2dm 3 / min. Then heat the material to 800℃ and keep the temperature constant for 2h. Protect the sample with inert gas until it cools down enough to be weighed.

[0045] Example 3

[0046] A method for oxidizing high-titanium slag, the method comprising:

[0047] First, weigh 30g of high titanium slag, the chemical composition of the slag is: ∑TiO2: 92.65%, S: 0.016%, P: 0.014%, C: 0.049% and ∑Fe: 5.26%. Grind the raw materials to a particle size of 425-600μm, then put the raw materials into a fluidized bed of a vertical tubular furnace, introduce liquefied protective gas Ar, keep the furnace temperature constant for 18 minutes, then replace the gas with an oxidizing mixed gas, the composition is 18% O2 and 18% H2O Ar, the mixed gas flow is controlled by a flow controller, the minimum is 2dm 3 / min. Then heat the material to 800℃ and keep the temperature constant for 2h. Protect the sample with inert gas until it cools down enough to be weighed.

[0048] Comparative Example 1

[0049] A method for oxidizing high-titanium slag, the method comprising:

[0050] First, weigh 30g of high titanium slag, the chemical composition of the slag is: ∑TiO2: 92.65%, S: 0.016%, P: 0.014%, C: 0.049% and ∑Fe: 5.26%. Grind the raw materials to a particle size of 425-600μm, then put the raw materials into a fluidized bed of a vertical tubular furnace, introduce protective gas Ar, keep the furnace temperature constant for 12 minutes, then replace the gas with an oxidizing mixed gas, the composition is 12% O2 Ar, the mixed gas flow is controlled by a flow controller, the minimum is 2dm 3 / min. Then heat the material to 800℃ and keep the temperature constant for 1h. Protect the sample with inert gas until it cools down enough to be weighed.

[0051] Comparative Example 2

[0052] A method for oxidizing high-titanium slag, the method comprising:

[0053] First, weigh 30g of high titanium slag, the chemical composition of the slag is: ∑TiO2: 92.65%, S: 0.016%, P: 0.014%, C: 0.049% and ∑Fe: 5.26%. Grind the raw materials to a particle size of 425-600μm, then put the raw materials into a fluidized bed of a vertical tubular furnace, introduce liquefied protective gas Ar, keep the furnace temperature constant for 15 minutes, then replace the gas with an oxidizing mixed gas, the composition is 15% O2 Ar, the mixed gas flow is controlled by a flow controller, the minimum is 2dm 3 / min. Then heat the material to 800℃ and keep the temperature constant for 2h. Protect the sample with inert gas until it cools down enough to be weighed.

[0054] Comparative Example 3

[0055] A method for oxidizing high-titanium slag, the method comprising:

[0056] First, weigh 30g of high titanium slag, the chemical composition of the slag is: ∑TiO2: 92.65%, S: 0.016%, P: 0.014%, C: 0.049% and ∑Fe: 5.26%. Grind the raw materials to a particle size of 425-600μm, then put the raw materials into a fluidized bed of a vertical tubular furnace, introduce liquefied protective gas Ar, keep the furnace temperature constant for 18 minutes, then replace the gas with an oxidizing mixed gas, the composition is 18% O2 Ar, the mixed gas flow is controlled by a flow controller, the minimum is 2dm 3 / min. Then heat the material to 800℃ and keep the temperature constant for 2h. Protect the sample with inert gas until it cools down enough to be weighed.

[0057] The weight gain rates of the products provided in each embodiment and comparative example are shown in the following table:

[0058]

[0059]

[0060] It can be seen from the above table that by comparing the data of Examples 1 to 3 and Comparative Examples 1 to 3, the weight gain rate of the product obtained by the method of introducing H2O in the atmosphere of heating and oxidation treatment is higher than the weight gain rate of the slag into which only oxygen is introduced under the same conditions, indicating that the introduction of H2O can increase the oxidation rate of high-titanium slag.

[0061] Various embodiments of the present application may be presented in the form of a range; it should be understood that the description in the form of a range is only for convenience and brevity, and should not be understood as a rigid limitation on the scope of the present application; therefore, the range description should be considered to have specifically disclosed all possible sub-ranges and single numerical values ​​within the range. For example, the range description from 1 to 6 should be considered to have specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5 and 6, which apply regardless of the range. In addition, whenever a numerical range is indicated herein, it is meant to include any cited number (fractional or integer) within the indicated range.

[0062] In the present application, in the absence of any contrary description, the directional words used, such as "upper" and "lower", are specifically the directions of the drawings in the accompanying drawings. In addition, in the description of the present specification, the terms "including", "comprising", etc. refer to "including but not limited to". In this article, relational terms such as "first" and "second" are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply that there is any such actual relationship or order between these entities or operations. In this article, "and / or" describes the association relationship of the associated objects, indicating that there may be three relationships, for example, A and / or B, which can represent: A exists alone, A and B exist at the same time, and B exists alone. Wherein A, B can be singular or plural. In this article, "at least one" refers to one or more, and "plural" refers to two or more. "At least one", "at least one of the following" or similar expressions refer to any combination of these items, including any combination of singular or plural items. For example, "at least one of a, b or c", or "at least one of a, b and c", can both mean: a, b, c, ab (i.e. a and b), ac, bc, or abc, where a, b and c can be single or multiple.

[0063] The above description is only a specific implementation of the present application, so that those skilled in the art can understand or implement the present application. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to the embodiments shown herein, but will conform to the widest range consistent with the principles and novel features applied for herein.

Claims

1. A method for oxidizing high-titanium slag, characterized in that: The method comprises: Obtaining high-titanium slag to be oxidized; The high-titanium slag is subjected to a heating oxidation treatment, wherein the atmosphere of the heating oxidation treatment includes H2O, and oxidation is completed to obtain a product.

2. The oxidation method of high titanium slag according to claim 1, characterized in that: In the atmosphere of the heating oxidation treatment, the volume proportion of H2O is 12% to 20%.

3. The oxidation method of high titanium slag according to claim 1, characterized in that: The atmosphere of the heating oxidation treatment is an oxygen-containing atmosphere.

4. The oxidation method of high titanium slag according to claim 1, characterized in that: In the atmosphere of the heating oxidation treatment, the volume proportion of O2 is 12% to 20%.

5. The oxidation method of high titanium slag according to claim 1, characterized in that: The atmosphere components of the heating oxidation treatment include, by volume fraction, 12% to 20% O2 and 12% to 20% H2O, with the remainder being inert gas and / or nitrogen.

6. The oxidation method of high titanium slag according to claim 5, characterized in that: The inert gas includes argon.

7. The oxidation method of high titanium slag according to claim 1, characterized in that: The particle size of the high titanium slag is 425 μm to 600 μm.

8. The oxidation method of high titanium slag according to claim 1, characterized in that: The temperature of the heating oxidation treatment is 700°C to 900°C.

9. The oxidation method of high titanium slag according to claim 1, characterized in that: The heating oxidation treatment time is 1h to 2h.

10. The oxidation method of high titanium slag according to claim 1, characterized in that: The flow rate of the heated oxidation treatment atmosphere is not less than 2dm 3 / min.

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