Method for preparing porous titanium dioxide catalyst carrier from ilmenite

Abstract

The invention provides a method for preparing a porous titanium dioxide catalyst carrier from ilmenite, and the porous titanium dioxide with high specific surface area, excellent adsorption performance and photocatalytic activity is prepared by selecting ilmenite with specific granularity and accurately controlling oxidation, reduction and acid leaching conditions. The method is simple to operate, mild in condition and environment-friendly, and provides a new way for preparation and application of porous titanium dioxide.

Description

Technical Field

[0001] The invention relates to the technical field of material preparation, in particular to a method for preparing porous titanium dioxide by utilizing ilmenite in a specific particle size range and controlling oxidation, reduction and acid leaching conditions.

[0002] Background technology: As a functional material, porous titanium dioxide has shown broad application prospects in many fields due to its unique physical and chemical properties. In particular, in the field of environmental protection, porous titanium dioxide can be used as an efficient adsorbent to remove heavy metal ions and organic pollutants from water. In the field of energy conversion and storage, porous titanium dioxide is widely used in devices such as solar cells, lithium-ion batteries and supercapacitors due to its high specific surface area and good photoelectric properties.

[0003] Traditional porous titanium dioxide has template method and sol-gel method. The precursors and template raw materials used in these methods are usually expensive and polluting, resulting in low yield. Therefore, it is necessary to further study environmentally friendly, low-cost and high-yield preparation methods to promote the widespread application of porous titanium dioxide in actual production and applications.

[0004] Therefore, developing a simple, environmentally friendly and economical method for preparing porous titanium dioxide has important practical significance. This method can not only reduce production costs and reduce environmental pollution, but also promote the application of porous titanium dioxide in more fields. By deeply studying the preparation technology of porous titanium dioxide and exploring new synthesis methods and process conditions, it is expected to provide a new way for the preparation and application of porous titanium dioxide. Summary of the invention

[0005] The present invention provides a method for preparing a porous titanium dioxide catalyst carrier from ilmenite. The method effectively prepares porous titanium dioxide by selecting ilmenite of a specific particle size and controlling the conditions of oxidation, reduction and acid leaching, and is easy for industrial production.

[0006] Specifically, the method of the present invention comprises the following steps:

[0007] 1. A method for preparing a porous titanium dioxide catalyst carrier from ilmenite, comprising the following steps:

[0008] S1. First, sieving ilmenite: selecting ilmenite with suitable particle size for sieving to obtain suitable ilmenite particles;

[0009] S2, air oxidation: the screened ilmenite particles are subjected to air oxidation treatment at high temperature to convert them into oxidized ilmenite;

[0010] S3, using hydrogen reduction: subjecting the oxidized ilmenite to hydrogen reduction treatment at high temperature to obtain an oxidized reduced ore;

[0011] S4, acid leaching: the redox ore is acid-leached at a temperature of 120-180°C using hydrochloric acid with a concentration of 15-30% under the condition of an acid-solid ratio of 5-10:1;

[0012] S5, washing and drying: washing the filter cake with 1.5-2.5wt% hydrochloric acid, and then washing with deionized water at a temperature of about 75°C until neutral; placing the washed filter cake in a blast drying oven, and drying at 105°C for 1.5-2.5h; obtaining a porous titanium dioxide catalyst carrier. Through the above method, porous titanium dioxide with high specific surface area, excellent adsorption performance and photocatalytic activity can be prepared.

[0013] Preferably, in step S1, the particle size is selected to be 50-300 mesh.

[0014] Preferably, in step S2, the high temperature condition is air oxidation treatment at a temperature of 600-900°C.

[0015] Preferably, in step S3, the high temperature condition is 600-800°C for hydrogen reduction treatment.

[0016] Preferably, in step S5, the hydrochloric acid washing filter cake is 2 wt%; and the drying time is 2 h.

[0017] Significant advantages of the method of the present invention

[0018] The method for preparing titanium dioxide provided by the present invention is not only simple to operate and mild in conditions, but also environmentally friendly, thus ensuring the sustainability of the production process. By precisely controlling the conditions of key steps such as oxidation, reduction and acid leaching, we are able to prepare porous titanium dioxide with excellent performance. This innovation not only enhances the application performance of titanium dioxide, but also provides more possibilities for its application in the fields of environmental protection, energy conversion and storage. This method not only optimizes the production process, but also reduces energy consumption and environmental pollution, making a positive contribution to the sustainable development of related industries. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order 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. 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 creative work.

[0020] Figure 1 This is the SEM image of the leached sample in Example 1.

[0021] Figure 2 This is a SEM image of the leached sample in Example 2.

[0022] In the following description, many specific details are set forth to facilitate a full understanding of the present invention, but the present invention may also be implemented in other ways different from those described herein, and those skilled in the art may make similar generalizations without violating the connotation of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below. DETAILED DESCRIPTION

[0023] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific implementation methods of the present invention are described in detail below in conjunction with the embodiments of the specification.

[0024] In the following description, many specific details are set forth to facilitate a full understanding of the present invention, but the present invention may also be implemented in other ways different from those described herein, and those skilled in the art may make similar generalizations without violating the connotation of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0025] Secondly, the term "one embodiment" or "embodiment" as used herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The term "in one embodiment" that appears in different places in this specification does not necessarily refer to the same embodiment, nor does it refer to a separate or selective embodiment that is mutually exclusive with other embodiments.

[0026] A method for preparing a porous titanium dioxide catalyst carrier from ilmenite, comprising the following steps:

[0027] S1. First, sieving ilmenite: selecting ilmenite with suitable particle size for sieving to obtain suitable ilmenite particles;

[0028] S2, air oxidation: the screened ilmenite particles are subjected to air oxidation treatment at high temperature to convert them into oxidized ilmenite;

[0029] S3, using hydrogen reduction: subjecting the oxidized ilmenite to hydrogen reduction treatment at high temperature to obtain an oxidized reduced ore;

[0030] S4, acid leaching: the redox ore is acid-leached at a temperature of 120-180°C using hydrochloric acid with a concentration of 15-30% under the condition of an acid-solid ratio of 5-10:1;

[0031] S5, washing and drying: washing the filter cake with 1.5-2.5wt% hydrochloric acid, and then washing with deionized water at a temperature of about 75°C until neutral; placing the washed filter cake in a blast drying oven, and drying at 105°C for 1.5-2.5h; obtaining a porous titanium dioxide catalyst carrier. Through the above method, porous titanium dioxide with high specific surface area, excellent adsorption performance and photocatalytic activity can be prepared.

[0032] Embodiment 1

[0033] Step 1: Screen the ilmenite ore through a screening device, and select the 100-200 mesh screened material as the raw material. Place the screened ilmenite in a blast drying oven and dry it at 105°C for 12 hours.

[0034] Step 2: Heat the muffle furnace to 750°C in advance. Place an alumina crucible containing 20.00 g of ilmenite accurately weighed in the center of the muffle furnace and start timing. After maintaining the temperature in the furnace for 45 minutes, take out the alumina crucible and place it in the air to cool naturally to room temperature.

[0035] Step 3: Place 120mL of 20% hydrochloric acid and 15g of accurately weighed oxide ore in a homogeneous reactor. Set the speed of the homogeneous reactor to 40r / min and start the heating program. When the temperature rises to 150°C, maintain this temperature for 8h. After the reactor cools down naturally, take out the reaction product and filter it. Wash the filter cake with 2wt% hydrochloric acid, and then wash it with deionized water at a temperature of about 75°C until it is neutral. Place the washed filter cake in a blast drying oven and dry it at 105°C for 2h to obtain the final product with a TiO2 content of 95.2%.

[0036] Embodiment 2

[0037] Step 1: Screen the ilmenite ore through a screening device, and select the 100-200 mesh screened material as the raw material. Place the screened ilmenite in a blast drying oven and dry it at 105°C for 12 hours.

[0038] Step 2: Heat the muffle furnace to 750°C in advance. Place an alumina crucible containing 20.00 g of ilmenite accurately weighed in the center of the muffle furnace and start timing. After maintaining the temperature in the furnace for 120 minutes, take out the alumina crucible and place it in the air to cool naturally to room temperature.

[0039] Step 3: Place an alumina crucible containing 20.00g of oxide ore accurately weighed in the center of the tube furnace. After setting the heating program, use argon as the protective gas during the heating process to ensure the purity of the furnace atmosphere. When the furnace temperature reaches 600°C, immediately switch the gas to hydrogen and maintain this temperature for 30 minutes to complete the reduction reaction. After the reaction is completed, quickly switch back to argon and continue to pass it in until the furnace temperature naturally cools to room temperature.

[0040] Step 4: Place 120mL of 20% hydrochloric acid and 15g of accurately weighed reduced ore in a homogeneous reactor. Set the speed of the homogeneous reactor to 40r / min and start the heating program. When the temperature rises to 150°C, maintain this temperature for 8h. After the reactor cools down naturally, take out the reaction product for filtration. Wash the filter cake with 2wt.% hydrochloric acid, and then wash it with deionized water at a temperature of about 75°C until it is neutral. Put the washed filter cake into a blast drying oven and dry it at 105°C for 2h. The TiO2 content is 94.5%.

[0041] Figure 1 , 2 The scanning electron microscope images of the cross-section of the sample after oxidation leaching of the screened ore in Example 1 and Example 2 respectively show the unique network structure of the sample after oxidation leaching of the screened ore.

Claims

1. A method for preparing a porous titanium dioxide catalyst carrier from ilmenite, characterized in that: The following steps are involved: S1. First, sieving ilmenite: selecting ilmenite with suitable particle size for sieving to obtain suitable ilmenite particles; S2, air oxidation: the screened ilmenite particles are subjected to air oxidation treatment at high temperature to convert them into oxidized ilmenite; S3, using hydrogen reduction: subjecting the oxidized ilmenite to hydrogen reduction treatment at high temperature to obtain an oxidized reduced ore; S4, acid leaching: the redox ore is acid-leached at a temperature of 120-180°C using hydrochloric acid with a concentration of 15-30% under the condition of an acid-solid ratio of 5-10:1; S5, washing and drying: washing the filter cake with 1.5-2.5wt% hydrochloric acid, and then washing with deionized water at a temperature of about 75°C until neutral; placing the washed filter cake in a forced air drying oven, and drying at 105°C for 1.5-2.5h; obtaining a porous titanium dioxide catalyst carrier.

2. A method for preparing a porous titanium dioxide catalyst carrier from ilmenite according to claim 1, characterized in that: In step S1, the particle size is selected to be 50-300 mesh.

3. A method for preparing a porous titanium dioxide catalyst carrier from ilmenite according to claim 1, characterized in that: In step S2, the high temperature condition is air oxidation treatment at a temperature of 600-900°C.

4. A method for preparing a porous titanium dioxide catalyst carrier from ilmenite according to claim 1, characterized in that: In step S3, the high temperature condition is 600-800°C for hydrogen reduction treatment.

5. A method for preparing a porous titanium dioxide catalyst carrier from ilmenite according to claim 1, characterized in that: In step S5, the filter cake is washed with 2 wt% hydrochloric acid and the drying time is 2 h.

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