Method for improving efficiency and purity of artificial rutile produced by reducing ilmenite corrosion

Abstract

The invention relates to the technical field of artificial rutile, and particularly discloses a method for improving the efficiency and purity of artificial rutile produced by reducing ilmenite rusting, and the method comprises the following steps: preparing a rusting solution from hydrochloric acid and industrial water, and injecting the rusting solution into a stirring rusting tank; injecting a catalyst into the stirring corrosion tank according to a set proportion; the reduced ilmenite is added into a stirring corrosion tank, meanwhile, ventilation is conducted through a Roots blower, a corrosion reaction is conducted, and hydrated iron oxide and artificial rutile slurry are generated; and separating the hydrated iron oxide from the artificial rutile slurry to obtain the artificial rutile. According to the method for improving the efficiency and purity of artificial rutile produced by reducing ilmenite rusting, the rusting reaction is rapidly and effectively carried out by adding the catalyst, the rusting reaction time is shortened to a great extent, the production efficiency is improved, and the energy consumption cost is saved; meanwhile, the catalyst, the rusting liquid and the washing liquid can be recycled, so that the cost of chemical reaction reagents is saved, and the pollution to the environment is reduced.

Description

Technical Field

[0001] The invention relates to the technical field of artificial rutile, and in particular to a method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion. Background Art

[0002] The main component of rutile is titanium dioxide, which is divided into natural rutile and artificial rutile. Natural rutile is scarce due to over-exploitation and is difficult to meet industrial needs. The composition of artificial rutile is the same as that of natural rutile. Most titanium ores in nature exist in the form of ilmenite (TiFeO3). To separate titanium dioxide from ilmenite, ilmenite needs to be reduced to reduced ilmenite, and then the reduced ilmenite is corroded to obtain artificial rutile.

[0003] The hydrochloric acid corrosion method currently widely used in the production of artificial rutile is hydrochloric acid corrosion. This involves adding reduced ilmenite to a corrosion solution containing hydrochloric acid. The iron in the reduced ilmenite reacts with the corrosion solution to form fine hydrated iron oxide particles, which are then removed from the ore. The hydrated iron oxide particles produced by the corrosion reaction are extremely fine, with most particles less than 20 microns in size. As the reaction proceeds, the number of iron oxide particles increases, and the hydrated iron oxide particles tend to adhere to the surface of the reduced ilmenite, reducing its contact with oxygen and the corrosion solution, slowing the corrosion reaction. This results in prolonged corrosion and high energy costs. Chinese patent application publication number CN114293031A discloses a multi-stage corrosion method for iron-containing minerals. The method includes detecting the slurry concentration and the iron content of the ore in a reaction tank, and then performing a multi-stage corrosion treatment on the iron-containing mineral based on the slurry concentration and the iron content of the ore. This multi-stage corrosion treatment can shorten the corrosion treatment time and improve production efficiency. However, this method requires monitoring the slurry concentration and performing multiple separation and feeding processes, which increases the operation process and complexity. To further improve production efficiency and reduce production costs, a method for improving the efficiency and purity of artificial rutile produced by corrosion of reduced ilmenite has been developed. Summary of the Invention

[0004] To address the above shortcomings, the present invention provides a method for improving the efficiency and purity of artificial rutile produced by reducing ilmenite through corrosion. This method overcomes the shortcomings of the hydrochloric acid corrosion method, accelerates the corrosion reaction, significantly shortens the corrosion reaction time, and reduces energy consumption costs. Furthermore, the catalyst is present in the recovered liquid and enters the recovery liquid pool, where it can circulate and participate in the corrosion reaction, thereby saving catalyst costs. The specific technical solution is as follows:

[0005] A method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, comprising the following steps:

[0006] (1) Prepare the corrosion solution: prepare the corrosion solution with hydrochloric acid and industrial water, and inject it into the stirring corrosion tank;

[0007] (2) preparing a catalyst: injecting a catalyst into a stirring corrosion tank, wherein the catalyst comprises one or two of an organic acid solution and a fatty alcohol polyoxyethylene ether; the organic acid is one or more of formic acid, acetic acid, and propionic acid;

[0008] (3) adding the reduced ilmenite into the stirring corrosion tank and simultaneously using a Roots blower for ventilation to carry out the corrosion reaction and generate hydrated iron oxide and artificial rutile slurry;

[0009] (4) using a cyclone and a high-frequency vibrating screen to separate the hydrated iron oxide and the artificial rutile slurry into an artificial rutile semi-finished product and iron red liquid;

[0010] (5) Washing and drying the artificial rutile semi-finished product to obtain an artificial rutile product.

[0011] The corrosion reaction mechanism of reduced ilmenite is as follows: the reduced ilmenite undergoes an electrochemical reaction in an acidic solution containing chloride ions, as shown in Equation (1). The Fe in the reduced ilmenite is converted to Fe₂O₃·H₂O, thereby removing a large amount of Fe from the reduced ilmenite and producing artificial rutile with a low Fe content. Titanium originally exists in the ore particles as titanium oxide. The corrosion reaction simply removes non-titanium impurities, primarily iron, resulting in artificial rutile composed primarily of titanium oxide.

[0012] Fe-2e - =Fe 2+

[0013] O2+2e - =O 2-

[0014] O2+2H2O+4e - =4OH -

[0015] Fe 2+ +2OH - =Fe(OH)2

[0016] 2Fe(OH)2+1 / 2O2=Fe2O3·H2O+H2O (1)

[0017] The inventors of the present invention discovered during their exploratory research that adding a catalyst to the corrosion system of reduced ilmenite and hydrochloric acid solution can enable the corrosion reaction to proceed quickly and effectively, greatly shortening the corrosion reaction time. The reason for this is analyzed as follows: adding a catalyst to the corrosion reaction system will generate a large number of bubbles, and a large number of fine hydrated iron oxide particles produced by the reaction will adhere to the surface of the bubbles, thereby reducing the probability of contact between the fine hydrated iron oxide and the surface of the reduced ilmenite, promoting the continuous and efficient reaction of the reduced ilmenite, thereby shortening the reaction time, improving production efficiency and saving energy consumption costs.

[0018] Preferably, in the above-mentioned method for improving the efficiency and purity of producing artificial rutile by corrosion of reduced ilmenite, the mass percentage concentration of HCl in the corrosion solution is 0.3% to 2%, and the mass ratio of the corrosion solution to the reduced ilmenite is 1.5 to 3:1.

[0019] Preferably, in the above-mentioned method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, the mass percentage concentration of the organic acid solution is 36% to 99.9%, the amount of the organic acid solution is 0.35 to 1.00% of the mass of the reduced ilmenite, and the amount of the fatty alcohol polyoxyethylene ether is 0.03 to 0.08% of the mass of the reduced ilmenite.

[0020] Preferably, in the above-mentioned method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, the catalyst is an acetic acid solution and a fatty alcohol polyoxyethylene ether, the acetic acid solution is used in an amount of 0.15-0.3% by mass of the reduced ilmenite, and the fatty alcohol polyoxyethylene ether is used in an amount of 0.005-0.02% by mass of the reduced ilmenite. The fatty alcohol polyoxyethylene ether and acetic acid work together to enhance the catalytic effect, further shorten the corrosion reaction time, and improve the corrosion efficiency.

[0021] Preferably, in the above method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, in step (3), the corrosion temperature is 40°C to 90°C, air is introduced, and the ventilation volume is 1200m 3 / h~1800m 3 / h, stirring speed is 70r / min~145r / min.

[0022] Preferably, in the above method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, the fatty alcohol polyoxyethylene ether is AEO-9, AEO-10 or AEO-12.

[0023] Preferably, in the above-mentioned method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, the artificial rutile obtained in step (5) is subjected to impurity removal, and the impurity removal method comprises the following steps:

[0024] S1. The artificial rutile semi-finished product obtained in step (5) is added to an acid leaching tank, an activator is added, the solid-liquid ratio is 1:4 to 6, and then activated at 110 to 130 ° C for 30 to 40 min;

[0025] S2. The activated artificial rutile obtained in step S1 is mixed with the mixed acid solution at a solid-liquid ratio of 1:4 to 6 and stirred at 90 to 100 ° C for 30 to 40 min;

[0026] S3. The artificial rutile obtained in step S2 is mixed with a mixed solution of hydrogen peroxide and sulfuric acid at a solid-to-liquid ratio of 1:4-6, stirred at 70-80°C for 30-40 minutes, filtered, washed, and dried to obtain a high-purity artificial rutile product. By optimizing the impurity removal steps and process parameters using the above impurity removal method, the purity of the artificial rutile can be increased to over 92%.

[0027] The washing liquid generated during the impurity removal process can be recycled and reused, but when the artificial rutile product is unqualified, the recycling will be stopped. At this time, the washing liquid needs to be regenerated. The acid leaching washing liquid is neutralized with lime milk to a pH of 7-8, and the recovered Fe(OH)3 and Al(OH)3 can be used as raw materials for building materials.

[0028] Preferably, in the above-mentioned method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, in step S1, the activator is sulfuric acid or sodium hydroxide solution, wherein the mass percentage concentration of sulfuric acid is 40-80%, and the mass percentage concentration of sodium hydroxide is 30-40%.

[0029] Preferably, in the above-mentioned method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, in step S2, the mixed acid solution is a mixed solution of sulfuric acid and nitric acid, wherein the mass percentage concentration of sulfuric acid is 15% and the mass percentage concentration of nitric acid is 3-5%.

[0030] Preferably, in the above method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, in step S3, the mass percentage concentration of hydrogen peroxide in the mixed solution of hydrogen peroxide and sulfuric acid is 3%, and the mass percentage concentration of sulfuric acid is 5%.

[0031] Preferably, the above-mentioned method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion also includes filtering the iron red liquid in step (4) and the washing liquid obtained by washing in step (5) to obtain an iron red filter cake and a corrosion recovery liquid, and the corrosion recovery liquid is collected in a corrosion recovery liquid pool for recycling in the corrosion reaction.

[0032] Compared with the prior art, the present invention has the following beneficial effects:

[0033] 1. In the method of the present invention for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, the addition of a catalyst allows the hydrochloric acid corrosion reaction to proceed rapidly and effectively, greatly shortening the corrosion reaction time, improving production efficiency, and saving energy costs. At the same time, the catalyst and corrosion solution of the present invention can be recycled, saving the cost of chemical reaction reagents and reducing environmental pollution.

[0034] 2. In the method of the present invention for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, the artificial rutile semi-finished product is further activated by adding sulfuric acid or sodium hydroxide solution, acid leaching with mixed acid, and oxidation with hydrogen peroxide. Impurities in the artificial rutile semi-finished product are removed by optimizing the impurity removal steps and process parameters, which can increase the purity of the artificial rutile product to above 92%. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] To more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for describing the embodiments. Obviously, the drawings described below are some embodiments of the present invention, and those skilled in the art can derive other drawings based on these drawings without inventive effort.

[0036] Figure 1 This is a process flow chart of the method for improving the efficiency of reducing ilmenite corrosion to produce artificial rutile according to the present invention;

[0037] Figure 2 This is a flow chart of the impurity removal process in the method of improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion according to the present invention. DETAILED DESCRIPTION

[0038] The specific embodiments of the present invention are described in detail below, but it should be understood that the scope of protection of the present invention is not limited by the specific embodiments. Unless otherwise defined, all technical terms used hereinafter have the same meaning as those generally understood by those skilled in the art. The technical terms used herein are only for the purpose of describing specific embodiments and are not intended to limit the scope of protection of the present invention. Unless otherwise specified, the various raw materials, reagents, instruments and equipment used in the present invention can be purchased from the market or can be prepared by existing methods.

[0039] The reduced ilmenite in the following examples and comparative examples comes from an ilmenite reduction process, and its main components (by mass percentage) include: titanium dioxide TiO2 61.25% and total iron TFe 31.56%.

[0040] Example 1

[0041] A method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion Figure 1 As shown, the following steps are included:

[0042] (1) Preparation of corrosion solution: hydrochloric acid and industrial water are used to prepare corrosion solution with a mass percentage concentration of 2% HCl, and the corrosion solution with a mass of 2 times that of the reduced ilmenite is injected into the stirring corrosion tank;

[0043] (2) Preparation of catalyst: Take 99.9% acetic acid solution as catalyst, the amount of acetic acid solution is 0.35% of the mass of the reduced ilmenite, and inject the acetic acid aqueous solution into the stirring corrosion tank;

[0044] (3) Add the reduced ilmenite into the stirring corrosion tank and use a Roots blower to introduce air at a ventilation volume of 1800m 3 / h, a stirring speed of 120r / min, a corrosion temperature of 81°C, and a corrosion reaction to obtain a slurry of hydrated iron oxide and artificial rutile;

[0045] (4) using a cyclone and a high-frequency vibrating screen to separate the hydrated iron oxide and the artificial rutile slurry into an artificial rutile semi-finished product and iron red liquid;

[0046] (5) washing the artificial rutile semi-finished product with water or washing recovery liquid, and drying it to obtain an artificial rutile product.

[0047] The iron red liquid in step (4) and the washing liquid obtained by washing in step (5) are subjected to filter pressing to obtain iron red filter cake and rust recovery liquid, and the rust recovery liquid is collected in a rust recovery liquid pool for recycling in the rust reaction.

[0048] 14 tons of reduced ilmenite was placed in a corrosion tank for corrosion according to the method of Example 1. The corrosion reaction took 8 hours to complete. The main components of the obtained artificial rutile (mass percentage) were: TiO2 83.85% and TFe 6.83%. The specific composition is shown in Table 1.

[0049] Example 2

[0050] A method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, comprising the following steps:

[0051] (1) Preparation of corrosion solution: hydrochloric acid and industrial water are used to prepare corrosion solution with a mass percentage concentration of 2% HCl, and the corrosion solution with a mass of 2 times that of the reduced ilmenite is injected into the stirring corrosion tank;

[0052] (2) Preparation of catalyst: Take 36% acetic acid aqueous solution as catalyst, the amount of acetic acid aqueous solution is 1.00% of the mass of the reduced ilmenite, and inject it into the stirring corrosion tank;

[0053] (3) Add the reduced ilmenite into the stirring corrosion tank and use a Roots blower to introduce air at a ventilation volume of 1200m 3 / h, the stirring speed is 120r / min, the corrosion temperature is 75°C, and the corrosion reaction is carried out to obtain hydrated iron oxide and artificial rutile slurry;

[0054] (4) using a cyclone and a high-frequency vibrating screen to separate the hydrated iron oxide and the artificial rutile slurry into an artificial rutile semi-finished product and iron red liquid;

[0055] (5) Washing the artificial rutile semi-finished product with water or washing recovery liquid and drying it to obtain artificial rutile.

[0056] The iron red liquid in step (4) and the washing liquid obtained by washing in step (5) are subjected to filter pressing to obtain iron red filter cake and rust recovery liquid, and the rust recovery liquid is collected in a rust recovery liquid pool for recycling in the rust reaction.

[0057] 14 tons of reduced ilmenite was placed in a corrosion tank for corrosion. According to the method of this embodiment, the corrosion reaction took 8 hours. The main components (mass percentage) of the obtained artificial rutile were: TiO2 83.96%, TFe 6.74%.

[0058] Example 3

[0059] A method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, comprising the following steps:

[0060] (1) Preparation of corrosion solution: hydrochloric acid and industrial water are used to prepare corrosion solution with a mass percentage concentration of 2% HCl, and the corrosion solution with a mass of 2 times that of the reduced ilmenite is injected into the stirring corrosion tank;

[0061] (2) Preparation of catalyst: Fatty alcohol polyoxyethylene ether AEO-10 is used as a catalyst, the amount of fatty alcohol polyoxyethylene ether AEO-10 is 0.05% of the mass of the reduced ilmenite, and is injected into the stirring corrosion tank;

[0062] (3) Add the reduced ilmenite into the stirring corrosion tank and use a Roots blower to introduce air at a ventilation volume of 1500m 3 / h, a stirring speed of 140r / min, a corrosion temperature of 75°C, and a corrosion reaction to obtain a hydrated iron oxide and artificial rutile slurry;

[0063] (4) using a cyclone and a high-frequency vibrating screen to separate the hydrated iron oxide and the artificial rutile slurry into an artificial rutile semi-finished product and iron red liquid;

[0064] (5) Washing the artificial rutile semi-finished product with water or washing recovery liquid and drying it to obtain artificial rutile.

[0065] The iron red liquid in step (4) and the washing liquid obtained by washing in step (5) are subjected to filter pressing to obtain iron red filter cake and rust recovery liquid, and the rust recovery liquid is collected in a rust recovery liquid pool for recycling in the rust reaction.

[0066] 14 tons of reduced ilmenite was placed in a corrosion tank for corrosion. According to the method of this embodiment, the corrosion reaction took 10.5 hours. The main components (mass percentage) of the obtained artificial rutile were: TiO2 83.27%, TFe 7.49%.

[0067] Example 4

[0068] A method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, comprising the following steps:

[0069] (1) Preparation of corrosion solution: hydrochloric acid and industrial water are used to prepare corrosion solution with a mass percentage concentration of 2% HCl, and the corrosion solution with a mass of 2 times that of the reduced ilmenite is injected into the stirring corrosion tank;

[0070] (2) Preparation of catalyst: Take 99.9% by mass acetic acid solution and fatty alcohol polyoxyethylene ether AEO-10 as catalysts, the amount of acetic acid aqueous solution is 0.25% by mass of the reduced ilmenite, and the amount of fatty alcohol polyoxyethylene ether AEO-10 is 0.01% by mass of the reduced ilmenite, and inject the acetic acid aqueous solution and fatty alcohol polyoxyethylene ether AEO-10 into the stirring corrosion tank in sequence;

[0071] (3) Add the reduced ilmenite into the stirring corrosion tank and use a Roots blower to introduce air at a ventilation volume of 1200m 3 / h, the stirring speed is 120r / min, the corrosion temperature is 75°C, and the corrosion reaction is carried out to obtain hydrated iron oxide and artificial rutile slurry;

[0072] (4) separating the hydrated iron oxide and artificial rutile slurry into artificial rutile and iron red liquid using a cyclone and a high-frequency vibrating screen;

[0073] (5) Washing the artificial rutile with water or a washing recovery liquid and drying the same to obtain the artificial rutile.

[0074] The iron red liquid in step (4) and the washing liquid obtained by washing in step (5) are subjected to filter pressing to obtain iron red filter cake and rust recovery liquid, and the rust recovery liquid is collected in a rust recovery liquid pool for recycling in the rust reaction.

[0075] 14 tons of reduced ilmenite was placed in a corrosion tank for corrosion. According to the method of this embodiment, the corrosion reaction took 7 hours to complete. The main components (mass percentage) of the obtained artificial rutile were: TiO2 84.02% and TFe 6.67%.

[0076] Comparative Example 1

[0077] A method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, comprising the following steps:

[0078] (1) Preparation of corrosion solution: prepare corrosion solution with HCl mass percentage concentration of 2% by hydrochloric acid and industrial water, and inject the corrosion solution with twice the concentration of reduced ilmenite into the stirring corrosion tank;

[0079] (3) Add the reduced ilmenite into the stirring corrosion tank and use a Roots blower to introduce air at a ventilation volume of 1800m 3 / h, a stirring speed of 120r / min, a corrosion temperature of 81°C, and a corrosion reaction to obtain a slurry of hydrated iron oxide and artificial rutile;

[0080] (4) using a cyclone and a high-frequency vibrating screen to separate the hydrated iron oxide and the artificial rutile slurry into an artificial rutile semi-finished product and iron red liquid;

[0081] (5) washing the artificial rutile semi-finished product with water or washing recovery liquid and then treating it to obtain artificial rutile.

[0082] In production, 14 tons of reduced ilmenite was placed in a corrosion tank for corrosion according to the method of Example 1. The corrosion reaction took 12 hours and was completed. The main components (mass percentage) of the obtained artificial rutile were: TiO2 82.30%, TFe 8.25%.

[0083] Comparative Example 2

[0084] This comparative example differs from Example 1 in that, in step (2), the amount of acetic acid solution used is 0.175% of the mass of the reduced ilmenite. The other steps and parameters are the same as in Example 1. The corrosion reaction in this comparative example takes 10 hours to complete, and the main components (mass percentage) of the resulting artificial rutile are: TiO2 83.72% and TFe 7.01%.

[0085] Comparative Example 3

[0086] This comparative example differs from Example 2 in that, in step (2), the amount of aqueous acetic acid used is 1.25% by mass of the reduced ilmenite. The other steps and parameters are the same as in Example 1. The corrosion reaction in this comparative example takes 8 hours to complete, and the main components (mass percentage) of the resulting artificial rutile are: TiO2 83.87% and TFe 6.79%.

[0087] In summary, the present invention uses a catalyst to shorten the corrosion reaction time, improve production efficiency, reduce energy consumption costs, and obtain artificial rutile with a purity of more than 82% through corrosion.

[0088] Example 5

[0089] The artificial rutile prepared in Example 1 was fed into an acid leaching tank and subjected to activation, acid leaching, and oxidation treatment to remove impurities. The impurity removal method comprises the following steps:

[0090] S1. The artificial rutile obtained in step (5) was added to an acid leaching tank, and a sulfuric acid solution was added as an activator, the mass percentage concentration of sulfuric acid was 40%, the solid-liquid ratio was 1:4, and then activated at 130 ° C for 30 min and filtered;

[0091] S2. The artificial rutile activated in step S1 was mixed with a mixed acid solution (sulfuric acid concentration of 15% by mass, nitric acid concentration of 5% by mass) at a solid-liquid ratio of 1:6, stirred at 100 ° C for 0.5h, and filtered;

[0092] S3. The artificial rutile obtained in step S2 was mixed with a mixed solution of 3% hydrogen peroxide and 5% sulfuric acid at a solid-liquid ratio of 1:5, stirred at 80°C for 0.5h, filtered, washed, and dried to obtain a high-purity artificial rutile product.

[0093] Example 6

[0094] The artificial rutile prepared in Example 1 was fed into an acid leaching tank and subjected to activation, acid leaching, and oxidation treatment to remove impurities. The impurity removal method comprises the following steps:

[0095] S1. The artificial rutile obtained in step (5) was added to an acid leaching tank, and a sulfuric acid solution was added as an activator, the mass percentage concentration of sulfuric acid was 55%, the solid-liquid ratio was 1:5, and then activated at 120 ° C for 40 min and filtered;

[0096] S2. The artificial rutile activated in step S1 was mixed with a mixed acid solution (sulfuric acid having a mass percentage concentration of 15% and nitric acid having a mass percentage concentration of 4%) at a solid-liquid ratio of 1:5, stirred at 90 ° C for 40 min, and filtered;

[0097] S3. The artificial rutile obtained in step S2 was mixed with a mixed solution of 3% hydrogen peroxide and 5% sulfuric acid at a solid-liquid ratio of 1:5, stirred at 70°C for 30min, filtered, washed, and dried to obtain a high-purity artificial rutile product.

[0098] Example 7

[0099] The artificial rutile prepared in Example 1 was fed into an acid leaching tank and subjected to activation, acid leaching, and oxidation treatment to remove impurities. The impurity removal method comprises the following steps:

[0100] S1. The artificial rutile obtained in step (5) was added to an acid leaching tank, an activator sodium hydroxide solution was added, the mass percentage concentration of sodium hydroxide was 35%, the solid-liquid ratio was 1:5, and then activated at 120 ° C for 30 min and filtered;

[0101] S2. The artificial rutile activated in step S1 was mixed with a mixed acid solution (sulfuric acid having a mass percentage concentration of 15% and nitric acid having a mass percentage concentration of 5%) at a solid-liquid ratio of 1:5, stirred at 90 ° C for 40 min, and filtered;

[0102] S3. The artificial rutile obtained in step S2 was mixed with a mixed solution of 3% hydrogen peroxide and 5% sulfuric acid at a solid-liquid ratio of 1:5, stirred at 70°C for 30min, filtered, washed, and dried to obtain a high-purity artificial rutile product.

[0103] The main chemical components (mass percentage) of the high-purity artificial rutile obtained by removing impurities in Examples 5 to 7 are shown in Table 1. As can be seen from the table, the purity of the artificial rutile can be increased to above 92% by further removing impurities in the present invention.

[0104] Table 1 Main chemical compositions of high-purity artificial rutile obtained by removing impurities in Examples 5 to 7

[0105] Main ingredients Before impurities removal Example 5 Example 6 Example 7 <![CDATA[TiO2(%)]]> 83.85 92.66 93.18 92.53 TFe (%) 6.83 1.55 1.36 1.79 CaO (%) 0.23 0.10 0.08 0.12 MgO (%) 0.46 0.18 0.15 0.23 MnO (%) 2.02 0.65 0.62 0.71 <![CDATA[Al2O3(%)]]> 1.20 0.42 0.37 0.40 P(％) 0.02 ＜0.01 ＜0.01 ＜0.01 S(％) 0.02 ＜0.01 ＜0.01 ＜0.01

[0106] The foregoing descriptions of specific exemplary embodiments of the present invention are for purposes of illustration and description. These descriptions are not intended to limit the invention to the precise forms disclosed, and it is apparent that many variations and modifications are possible in light of the foregoing teachings. The exemplary embodiments have been selected and described for the purpose of explaining the specific principles of the invention and their practical application, thereby enabling those skilled in the art to realize and utilize a variety of exemplary embodiments of the invention and various options and modifications. The scope of the invention is intended to be defined by the claims and their equivalents.

Claims

1. A method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion, characterized in that: The following steps are involved: (1) Prepare the corrosion solution: prepare the corrosion solution with hydrochloric acid and industrial water, and inject it into the stirring corrosion tank; (2) preparing a catalyst: injecting a catalyst into a stirring corrosion tank, wherein the catalyst comprises one or two of an organic acid solution and a fatty alcohol polyoxyethylene ether; the organic acid is one or more of formic acid, acetic acid, and propionic acid; (3) adding the reduced ilmenite into the stirring corrosion tank and simultaneously using a Roots blower for ventilation to carry out the corrosion reaction and generate hydrated iron oxide and artificial rutile slurry; (4) using a cyclone and a high-frequency vibrating screen to separate the hydrated iron oxide and the artificial rutile slurry into an artificial rutile semi-finished product and iron red liquid; (5) Washing and drying the artificial rutile semi-finished product to obtain an artificial rutile product.

2. The method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion according to claim 1, characterized in that: The mass percentage concentration of HCl in the corrosion solution is 0.3% to 2%, and the mass ratio of the corrosion solution to the reduced ilmenite is 1.5 to 3:

1.

3. The method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion according to claim 1, characterized in that: The mass percentage concentration of the organic acid solution is 36% to 99.9%, and the amount of the organic acid solution is 0.35 to 1.00% of the mass of the reduced ilmenite; the amount of the fatty alcohol polyoxyethylene ether is 0.03 to 0.08% of the mass of the reduced ilmenite.

4. The method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion according to claim 1, characterized in that: The catalyst is acetic acid solution and fatty alcohol polyoxyethylene ether. The amount of the acetic acid solution is 0.15-0.3% of the mass of the reduced ilmenite, and the amount of the fatty alcohol polyoxyethylene ether is 0.005-0.02% of the mass of the reduced ilmenite.

5. The method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion according to claim 1, characterized in that: The fatty alcohol polyoxyethylene ether is AEO-9, AEO-10 or AEO-12.

6. The method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion according to claim 1, characterized in that: In the step (3), the corrosion temperature is 40℃~90℃, air is introduced, and the ventilation volume is 1200m 3 / h~1800m 3 / h, stirring speed is 70r / min~145r / min.

7. The method for improving the efficiency of producing artificial rutile by reducing ilmenite corrosion according to claim 1, characterized in that: The artificial rutile obtained in step (5) is subjected to impurity removal, and the impurity removal method comprises the following steps: S1. The artificial rutile obtained in step (5) is added to an acid leaching tank, an activator is added, the solid-liquid ratio is 1:4 to 6, and then activated at 110 to 130 ° C for 30 to 40 min; S2. The activated artificial rutile obtained in step S1 is mixed with the mixed acid solution at a solid-liquid ratio of 1:4 to 6 and stirred at 90 to 100 ° C for 30 to 40 min; S3. The artificial rutile obtained in step S2 is mixed with a mixed solution of hydrogen peroxide and sulfuric acid at a solid-liquid ratio of 1:4 to 6, stirred at 70 to 80°C for 30 to 40 minutes, filtered, washed, and dried to obtain a high-purity artificial rutile product.

8. The method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion according to claim 7, characterized in that: In step S1, the activator is sulfuric acid or sodium hydroxide solution, wherein the mass percentage concentration of sulfuric acid is 40-80%, and the mass percentage concentration of sodium hydroxide is 30-40%; in step S2, the mixed acid solution is a mixed solution of sulfuric acid and nitric acid, wherein the mass percentage concentration of sulfuric acid is 15%, and the mass percentage concentration of nitric acid is 3-5%.

9. The method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion according to claim 7, characterized in that: In step S3, the mass percentage concentration of hydrogen peroxide in the mixed solution of hydrogen peroxide and sulfuric acid is 3%, and the mass percentage concentration of sulfuric acid is 5%.

10. The method for improving the efficiency and purity of producing artificial rutile by reducing ilmenite corrosion according to claim 1, characterized in that: The method further comprises filtering the iron red liquid in step (4) and the washing liquid obtained by washing in step (5) to obtain an iron red filter cake and a rust recovery liquid, and collecting the rust recovery liquid in a rust recovery liquid pool for recycling in the rust reaction.

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