Method for preparing artificial rutile and recycling mother liquor of artificial rutile

Abstract

The invention discloses a method for preparing artificial rutile and recycling mother liquor of the artificial rutile, which comprises the following steps of: performing high-temperature oxidizing roasting treatment on the mother liquor of the artificial rutile by using titanium slag coal gas to obtain diluted hydrochloric acid and by-products; the by-product is mixed with titanium concentrate and a reducing agent to form a first mixture, the first mixture is subjected to mixed smelting, and a titanium raw material product and titanium slag coal gas are obtained; the titanium slag coal gas generated by mixed smelting is reused for high-temperature oxidizing roasting treatment; wherein the artificial rutile mother liquor is mother liquor generated in an acid leaching step in artificial rutile production. Diluted hydrochloric acid and by-products generated by surplus titanium slag electric furnace gas and artificial rutile mother liquor are recycled, waste of gas resources is avoided, the problem that the treatment cost of the artificial rutile mother liquor is high is effectively solved, meanwhile, the by-products and titanium concentrate are added into the electric furnace to be smelted, the titanium efficiency is improved, and the additional value of iron is improved.

Description

Technical Field

[0001] The invention relates to the technical field of artificial rutile production, and in particular to a method for preparing artificial rutile and recycling its mother liquor. Background Art

[0002] Artificial rutile mother liquor is a waste liquid generated in the process of producing artificial rutile. In some production processes, such as the hydrochloric acid method for preparing artificial rutile, a large amount of artificial rutile mother liquor will be produced. This mother liquor has some characteristics, such as containing a certain concentration of acid (such as hydrochloric acid) and other chemical components, which may include iron ions, etc. If it is discharged directly, it will pollute the environment and the useful components in it will be wasted. In order to solve these problems and realize the comprehensive utilization of resources and environmental protection. It is of great significance to carry out research on the recycling of artificial rutile mother liquor.

[0003] Based on this, the existing technology still needs to be improved. Summary of the invention

[0004] In order to solve the above technical problems, the embodiment of the present invention proposes a method for preparing artificial rutile and recycling its mother liquor, so as to solve the problem of mother liquor treatment in the artificial rutile production process in the prior art.

[0005] In order to solve the above technical problems, on the one hand, some embodiments of the present invention disclose a method for recycling artificial rutile mother liquor, comprising: Step 1: using titanium slag gas to perform high-temperature oxidation roasting on artificial rutile mother liquor to obtain dilute hydrochloric acid and by-products; Step 2: Mixing the by-product with titanium concentrate and a reducing agent to form a first mixture, and performing mixed smelting on the first mixture to obtain a titanium raw material product and titanium slag gas; Step 3: The titanium slag gas produced by the mixed smelting is recycled to step 1; The artificial rutile mother liquor is the mother liquor produced in the acid leaching step in the production of artificial rutile. In some embodiments, the by-product includes ferric oxide, and the amount of the by-product added is 5%-15% of the total mass of the first mixture.

[0006] In some embodiments, the dilute hydrochloric acid obtained in step 1 is recycled for leaching titanium concentrate to prepare artificial rutile.

[0007] In some embodiments, the amount of titanium slag gas required to process the artificial rutile mother liquor produced by producing one ton of artificial rutile is 1500-3000m 3 .

[0008] In some embodiments, the mixed smelting in step 2 is carried out in an electric furnace.

[0009] In some embodiments, during the mixed smelting, the electric furnace smelting parameter control includes: The current-pressure ratio is 130-150; the current value range is 38000-45000A.

[0010] In some embodiments, the method further comprises: leaching the titanium concentrate with dilute hydrochloric acid and performing solid-liquid separation, and using the liquid phase as the artificial rutile mother liquor.

[0011] In some embodiments, the concentration of the dilute hydrochloric acid is 5%-22% by mass percentage.

[0012] On the other hand, an embodiment of the present invention further discloses a method for producing artificial rutile, which comprises: Step 1: Leaching the titanium concentrate with dilute hydrochloric acid and performing solid-liquid separation to obtain an artificial rutile mother liquor; Step 2: using titanium slag gas to perform high-temperature oxidation and burning treatment on the artificial rutile mother liquor to obtain dilute hydrochloric acid and by-products; Step 3: After the by-product is mixed with titanium concentrate and a reducing agent into a first mixture, mixed smelting is performed in a circuit to obtain a titanium raw material product and titanium slag gas; Step 4: Reuse the titanium slag gas in step 2, and reuse the dilute hydrochloric acid in step 1.

[0013] In some embodiments, the titanium raw material product includes titanium dioxide and iron monoxide, and, in terms of mass percentage, the titanium dioxide accounts for 74%-76% of the total amount of the titanium raw material product; the iron monoxide accounts for 8%-10% of the total amount of the titanium raw material product.

[0014] By adopting the above technical solution, the present invention has at least the following beneficial effects: The present invention provides a method for preparing artificial rutile and recycling its mother liquor, which allows the byproducts such as dilute hydrochloric acid and Fe2O3 produced by surplus titanium slag electric furnace gas and artificial rutile mother liquor to be recycled, eliminates the waste of gas resources, and effectively solves the problem of high treatment costs of artificial rutile mother liquor. At the same time, byproducts such as Fe2O3 containing certain impurity oxides and titanium concentrate are added to the electric furnace for smelting, which not only improves the titanium efficiency but also increases the added value of iron. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] In order to more clearly illustrate the embodiments of the present invention 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, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0016] Figure 1 The present invention is a flowchart of a method for preparing artificial rutile disclosed in some embodiments of the present invention. DETAILED DESCRIPTION

[0017] The following is a further detailed description of the embodiments of the present disclosure in conjunction with the accompanying drawings and examples. The detailed description of the following embodiments and the accompanying drawings are used to exemplarily illustrate the principles of the present disclosure, but cannot be used to limit the scope of the present disclosure. The present disclosure can be implemented in many different forms and is not limited to the specific embodiments disclosed herein, but includes all technical solutions that fall within the scope of the claims.

[0018] The present disclosure provides these embodiments to make the present disclosure thorough and complete, and to fully express the scope of the present disclosure to those skilled in the art. It should be noted that unless otherwise specifically stated, the relative arrangement of the parts and steps, the composition of the materials, the numerical expressions and the numerical values ​​set forth in these embodiments should be interpreted as being merely exemplary, and not as limiting.

[0019] It should be noted that, in the description of the present disclosure, unless otherwise specified, the meaning of "multiple" is greater than or equal to two; the terms "upper", "lower", "left", "right", "inner", "outer", etc., indicating the orientation or positional relationship, are only for the convenience of describing the present disclosure and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation of the present disclosure. When the absolute position of the object being described changes, the relative positional relationship may also change accordingly.

[0020] In addition, the words "first", "second" and similar words used in the present disclosure do not indicate any order, quantity or importance, but are only used to distinguish different parts. "Vertical" does not mean vertical in the strict sense, but is within the tolerance range. "Parallel" does not mean parallel in the strict sense, but is within the tolerance range. "Include" or "comprising" and similar words mean that the elements before the word include the elements listed after the word, and do not exclude the possibility of including other elements.

[0021] It should also be noted that in the description of the present disclosure, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be directly connected or indirectly connected through an intermediate medium. For ordinary technicians in this field, the specific meanings of the above terms in the present disclosure can be understood according to the specific circumstances. When a specific device is described as being located between a first device and a second device, there may or may not be an intermediate device between the specific device and the first device or the second device.

[0022] All terms used in the present disclosure have the same meanings as those understood by those of ordinary skill in the art to which the present disclosure belongs, unless otherwise specifically defined. It should also be understood that terms defined in general dictionaries, for example, should be interpreted as having meanings consistent with their meanings in the context of the relevant technology, and should not be interpreted in an idealized or extremely formal sense, unless explicitly defined as such herein.

[0023] Technologies, methods, and equipment known to ordinary technicians in the relevant art may not be discussed in detail, but where appropriate, the technologies, methods, and equipment should be considered part of the specification.

[0024] Some embodiments of the present invention disclose a method for recycling artificial rutile mother liquor, comprising: Step 1: Use titanium slag gas to perform high-temperature oxidation roasting on the artificial rutile mother liquor to obtain dilute hydrochloric acid and by-products; the by-products include ferric oxide, and the amount of the by-products added is 5%-15% of the total mass of the first mixture. At the same time, the dilute hydrochloric acid obtained in this step can be directly reused for leaching of titanium concentrate to prepare artificial rutile. Generally, the concentration of the dilute hydrochloric acid is 5%-22% in terms of mass percentage. The reused dilute hydrochloric acid needs to be concentrated or diluted so that its concentration is within the appropriate range to ensure the smooth progress of the leaching reaction.

[0025] Step 2: Mix the by-product with titanium concentrate and a reducing agent to form a first mixture, and perform mixed smelting on the first mixture in an electric furnace to obtain a titanium raw material product and titanium slag gas; during mixed smelting, the electric furnace smelting parameter control includes: flow pressure ratio 130-150; current value range is 38000-45000A.

[0026] Step 3: The titanium slag gas produced by the mixed smelting is recycled to step 1; The artificial rutile mother liquor is the mother liquor produced in the acid leaching step in the production of artificial rutile, that is, titanium concentrate is leached with dilute hydrochloric acid and the solid-liquid separation is carried out, and the liquid phase is used as the artificial rutile mother liquor.

[0027] Generally, the amount of titanium slag gas required to process the artificial rutile mother liquor produced by producing one ton of artificial rutile is 1500-3000m 3 .

[0028] The method for recycling artificial rutile mother liquor disclosed in the above embodiment allows the surplus titanium slag electric furnace gas and by-products such as dilute hydrochloric acid and Fe2O3 produced by the artificial rutile mother liquor to be recycled, eliminates the waste of gas resources, and effectively solves the problem of high treatment costs of artificial rutile mother liquor. At the same time, by-products such as Fe2O3 containing certain impurity oxides and titanium concentrate are added to the electric furnace for smelting, which not only improves the titanium efficiency, but also increases the added value of iron.

[0029] Some embodiments of the present invention also disclose a method for producing artificial rutile, which comprises: Step 1: Leaching the titanium concentrate with dilute hydrochloric acid and performing solid-liquid separation to obtain an artificial rutile mother liquor; Step 2: using titanium slag gas to perform high-temperature oxidation and burning treatment on the artificial rutile mother liquor to obtain dilute hydrochloric acid and by-products; Step 3: After mixing the by-product with titanium concentrate and a reducing agent into a first mixture, the mixed smelting is carried out in a circuit to obtain a titanium raw material product and titanium slag gas; wherein the titanium raw material product includes titanium dioxide and iron monoxide, and, in terms of mass percentage, the titanium dioxide accounts for 74%-76% of the total amount of the titanium raw material product; the iron monoxide accounts for 8%-10% of the total amount of the titanium raw material product.

[0030] Step 4: Reuse the titanium slag gas in step 2, and reuse the dilute hydrochloric acid in step 1.

[0031] The preparation method of artificial rutile disclosed in the above embodiment allows the by-products such as dilute hydrochloric acid and Fe2O3 produced by surplus titanium slag electric furnace gas and artificial rutile mother liquor to be recycled, eliminates the waste of gas resources, and effectively solves the problem of high treatment costs of artificial rutile mother liquor. At the same time, by-products such as Fe2O3 containing certain impurity oxides and titanium concentrate are added to the electric furnace for smelting, which not only improves the titanium efficiency, but also increases the added value of iron.

[0032] Example 1 like Figure 1 The method for preparing the artificial rutile shown comprises: The titanium concentrate was leached with dilute hydrochloric acid and solid-liquid separated to obtain 7.2 tons of artificial rutile mother liquor and 1 ton of artificial rutile; Utilize 1900m 3The artificial rutile mother liquor is subjected to high-temperature oxidation roasting treatment by titanium slag electric furnace gas. The dilute hydrochloric acid obtained after concentration-absorption can be used for leaching titanium concentrate to prepare artificial rutile. 1.05t of by-products such as Fe2O3 containing certain impurity oxides can also be obtained. It can be mixed with titanium concentrate and reducing agent and added into the electric furnace as the first mixture for smelting. The addition amount is 10% of the total mass of the first mixture. The electric furnace smelting operation parameters are adjusted, and the flow pressure is set to 135 and the current value is 40000A. Finally, a titanium raw material product suitable for sponge titanium and sulfuric acid titanium dioxide is obtained. In addition, the amount of electric furnace gas generated during the smelting process is greater than 1900m 3 , used to treat artificial rutile mother liquor, and the remaining electric furnace gas can be stored for backup. After testing, the obtained titanium raw material product has a mass percentage of TiO2 of 74% and FeO of 10%.

[0033] Example 2 like Figure 1 The method for preparing the artificial rutile shown comprises: The titanium concentrate was leached with dilute hydrochloric acid and solid-liquid separated to obtain 6.98 tons of artificial rutile mother liquor and 1.03 tons of artificial rutile; Utilize 1860m 3 The artificial rutile mother liquor is subjected to high-temperature oxidation roasting treatment by titanium slag electric furnace gas. The dilute hydrochloric acid obtained after concentration-absorption can be used for leaching titanium concentrate to prepare artificial rutile. 0.99t of by-products such as Fe2O3 containing certain impurity oxides can also be obtained. It can be mixed with titanium concentrate and reducing agent and added into the electric furnace as the first mixture for smelting. The addition amount is 8% of the total mass of the first mixture. The electric furnace smelting operation parameters are adjusted, and the flow pressure is set to 145 and the current value is 43000A. Finally, a titanium raw material product suitable for sponge titanium and sulfuric acid titanium dioxide is obtained. In addition, the amount of electric furnace gas generated during the smelting process is greater than 1860m 3 , used to treat artificial rutile mother liquor, and the remaining electric furnace gas can be stored for backup. After testing, the obtained titanium raw material product has a mass percentage of TiO2 of 76% and FeO of 8%.

[0034] Example 3 like Figure 1 The method for preparing the artificial rutile shown comprises: The titanium concentrate was leached with dilute hydrochloric acid and solid-liquid separated to obtain 7.23 tons of artificial rutile mother liquor and 1.13 tons of artificial rutile; Utilize 1960m 3The artificial rutile mother liquor is subjected to high-temperature oxidation roasting treatment by titanium slag electric furnace gas. The dilute hydrochloric acid obtained after concentration-absorption can be used for leaching titanium concentrate to prepare artificial rutile. 1.06t of by-products such as Fe2O3 containing certain impurity oxides can also be obtained. It can be mixed with titanium concentrate and reducing agent and added into the electric furnace as the first mixture for smelting. The addition amount is 15% of the total mass of the first mixture. The electric furnace smelting operation parameters are adjusted, and the flow pressure is set to 135 and the current value is 45000A. Finally, a titanium raw material product suitable for sponge titanium and sulfuric acid titanium dioxide is obtained. In addition, the amount of electric furnace gas generated during the smelting process is greater than 1960m 3 , used to treat artificial rutile mother liquor, and the remaining electric furnace gas can be stored for backup. After testing, the obtained titanium raw material product has a mass percentage of TiO2 of 75% and FeO of 9%.

[0035] Experiments have shown that every ton of artificial rutile produces about 7 tons of artificial rutile mother liquor, which requires 1800-2000m 3 Titanium slag is subjected to high temperature oxidation roasting treatment with electric furnace gas; about 1 t of by-products such as Fe2O3 can be obtained, which are added into the electric furnace at a mass percentage of 5%-15% together with titanium concentrate and a reducing agent mixture for smelting. By adjusting the electric furnace parameters such as: flow pressure ratio 135-145, current value 40000~42000A, titanium raw material products suitable for sponge titanium and sulfuric acid titanium dioxide (TiO2 is 74~76%, FeO is 8-10%) are finally obtained. At the same time, the amount of gas generated in the smelting process fully meets the gas demand for artificial rutile mother liquor.

[0036] To sum up, the method for preparing artificial rutile and recycling its mother liquor disclosed in the embodiment of the present invention allows the by-products such as dilute hydrochloric acid and Fe2O3 produced by surplus titanium slag electric furnace gas and artificial rutile mother liquor to be recycled, eliminates the waste of gas resources, and effectively solves the problem of high treatment costs of artificial rutile mother liquor. At the same time, by-products such as Fe2O3 containing certain impurity oxides and titanium concentrate are added to the electric furnace for smelting, which not only improves the titanium efficiency, but also increases the added value of iron.

[0037] So far, various embodiments of the present disclosure have been described in detail. In order to avoid obscuring the concept of the present disclosure, some details known in the art are not described. Based on the above description, those skilled in the art can fully understand how to implement the technical solution disclosed here.

[0038] Although some specific embodiments of the present disclosure have been described in detail by way of examples, it should be understood by those skilled in the art that the above examples are for illustration only and are not intended to limit the scope of the present disclosure. It should be understood by those skilled in the art that the above embodiments may be modified or some technical features may be replaced by equivalents without departing from the scope and spirit of the present disclosure. In particular, the various technical features mentioned in the various embodiments may be combined in any manner as long as there is no structural conflict.

Claims

1. A method for recycling artificial rutile mother liquor, characterized in that: include: Step 1: using titanium slag gas to perform high-temperature oxidation roasting on artificial rutile mother liquor to obtain dilute hydrochloric acid and by-products; Step 2: Mixing the by-product with titanium concentrate and a reducing agent to form a first mixture, and performing mixed smelting on the first mixture to obtain a titanium raw material product and titanium slag gas; Step 3: Reusing the titanium slag gas produced by the mixed smelting in step 1; Wherein, the artificial rutile mother liquor is the mother liquor produced in the acid leaching step in the production of artificial rutile.

2. The method for recycling artificial rutile mother liquor according to claim 1, characterized in that: The by-product includes ferric oxide, and the added amount of the by-product is 5%-15% of the total mass of the first mixture.

3. The method for recycling artificial rutile mother liquor according to claim 1, characterized in that: The dilute hydrochloric acid obtained in step 1 is recycled for leaching titanium concentrate to prepare artificial rutile.

4. The method for recycling artificial rutile mother liquor according to claim 1, characterized in that The amount of titanium slag gas required to process the artificial rutile mother liquor produced by producing one ton of artificial rutile is 1500-3000m 3 .

5. The method for recycling artificial rutile mother liquor according to claim 1, characterized in that: The mixed smelting in step 2 is carried out in an electric furnace.

6. The method for recycling artificial rutile mother liquor according to claim 5, characterized in that: During the mixed smelting, the electric furnace smelting parameter control includes: The current-pressure ratio is 130-150; the current value range is 38000-45000A.

7. The method for recycling artificial rutile mother liquor according to claim 1, characterized in that: Also includes: The titanium concentrate is leached with dilute hydrochloric acid and the solid-liquid separation is carried out, and the liquid phase is used as the artificial rutile mother liquor.

8. The method for recycling artificial rutile mother liquor according to claim 1, characterized in that: Calculated by mass percentage, the concentration of the dilute hydrochloric acid is 5%-22%.

9. A method for producing artificial rutile, characterized in that: include: Step 1: Leaching the titanium concentrate with dilute hydrochloric acid and performing solid-liquid separation to obtain an artificial rutile mother liquor; Step 2, using titanium slag gas to perform high-temperature oxidation and burning treatment on the artificial rutile mother liquor to obtain dilute hydrochloric acid and by-products; Step 3: After the by-product is mixed with titanium concentrate and a reducing agent into a first mixture, mixed smelting is performed in a circuit to obtain a titanium raw material product and titanium slag gas; Step 4: Reuse the titanium slag gas in step 2, and reuse the dilute hydrochloric acid in step 1.

10. The method for preparing artificial rutile according to claim 9, characterized in that: The titanium raw material product includes titanium dioxide and iron monoxide, and, in terms of mass percentage, the titanium dioxide accounts for 74%-76% of the total amount of the titanium raw material product; the iron monoxide accounts for 8%-10% of the total amount of the titanium raw material product.

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