Preparation method of small Fisher tantalum oxide

Abstract

The invention provides a preparation method of small Fisher tantalum oxide, and relates to the technical field of industrial small Fisher tantalum oxide preparation. The preparation method comprises the following steps: carrying out normal-temperature neutralization treatment on Ta2O5-containing industrial tantalum liquid by using stronger ammonia water, stirring and mixing, and carrying out solid-liquid separation to obtain a tantalum hydroxide filtrate; and sequentially carrying out drying treatment, calcining treatment and crushing and screening treatment on the tantalum hydroxide filtrate to obtain the small Fisher tantalum oxide. The preparation method of the small Fisher tantalum oxide, provided by the invention, has the remarkable beneficial effects of improving the production efficiency, reducing the cost, improving the product quality and improving the environmental sustainability.

Description

Technical Field

[0001] The invention relates to the technical field of industrial small Feehertz tantalum oxide preparation, and in particular to a method for preparing small Feehertz tantalum oxide. Background Art

[0002] As an important inorganic non-metallic material, tantalum oxide plays an important role in many fields due to its unique physical and chemical properties. This material is well-known for its high melting point, corrosion resistance, and good electrical and optical properties. It is widely used in catalysts, electronic materials, optical materials, biomedicine and other fields. Especially in the field of catalysts, tantalum oxide can effectively promote chemical reaction rates, improve selectivity and conversion rates due to its high specific surface area and excellent dispersibility. In the field of electronic materials, the application of tantalum oxide helps to improve the integration, response speed and energy storage capacity of devices. In terms of optical materials, tantalum oxide can be used to prepare optical films and display technologies with high transparency and low scattering, thereby improving display quality. In the field of biomedicine, the unique properties of tantalum oxide make it show potential application value in drug delivery, biosensing and other fields.

[0003] At present, the industrial method for preparing tantalum oxide mainly adopts hydrometallurgical technology, in which the fluorotantalate solution is neutralized with ammonia to generate tantalum hydroxide, and then tantalum oxide is generated through steps such as fluorine washing, drying, and calcination. In particular, small Fee's tantalum oxide, that is, tantalum oxide with an average particle size of less than 0.8 microns, exhibits better performance due to its ultra-small particle size. However, there are some defects in the existing preparation technology. The industrial tantalum liquid is diluted and neutralized with liquid ammonia. In this process, a relatively high neutralization temperature needs to be controlled, resulting in a large consumption of ammonia. In addition, the particle size of the prepared product is unstable and fluctuates in the range of 0.8 to 1 micron, which limits its potential for application in high-precision fields.

[0004] The existing technology also faces the problem of complex process in the process of preparing small Fee's tantalum oxide. The neutralization process requires dilution of industrial tantalum liquid, which not only increases production costs, but also may lead to a decrease in product purity. At the same time, due to the high control requirements of the neutralization temperature, the accuracy of the equipment and the skill requirements of the operator are also increased, which undoubtedly increases the difficulty and cost of production. On the whole, the existing technology has defects such as high ammonia consumption, unstable product particle size and complex process when preparing small Fee's tantalum oxide. These problems limit the further development of small Fee's tantalum oxide in high-end application fields.

[0005] In view of this, the present invention is proposed. Summary of the invention

[0006] The object of the present invention is to provide a method for preparing small Feehertz tantalum oxide, which has the advantages of low neutralization temperature requirement, small ammonia consumption, simple process and the like.

[0007] In order to achieve the above-mentioned purpose of the present invention, the following technical solutions are particularly adopted:

[0008] In a first aspect, the present invention provides a method for preparing small Fee-shaped tantalum oxide, comprising:

[0009] The industrial tantalum liquid containing Ta2O5 is neutralized at room temperature by concentrated ammonia water, and after solid-liquid separation, a tantalum hydroxide filtrate is obtained;

[0010] The tantalum hydroxide filtrate is sequentially subjected to drying treatment, calcination treatment and crushing and screening treatment to obtain small Fee's tantalum oxide.

[0011] In an optional embodiment, the concentration of Ta2O5 contained in the industrial tantalum liquid is 50g / L to 80g / L.

[0012] In an optional embodiment, the industrial tantalum liquid containing Ta2O5 is neutralized at room temperature using concentrated ammonia water, and after solid-liquid separation, a tantalum hydroxide filtrate is obtained, comprising:

[0013] Adding concentrated ammonia water to the industrial tantalum liquid and stirring and mixing, and performing a neutralization treatment at room temperature;

[0014] After stopping adding the concentrated ammonia solution, continue stirring and mixing to obtain a mixed solution;

[0015] The mixed liquid is subjected to solid-liquid separation to obtain the tantalum hydroxide filtrate.

[0016] In an optional embodiment, the concentrated ammonia water is 18% to 20% ammonia water.

[0017] In an optional embodiment, concentrated ammonia water is added to the industrial tantalum liquid and stirred to mix, and a neutralization treatment step is performed at room temperature. The pH of the industrial tantalum liquid after neutralization is 8-10.

[0018] In an optional embodiment, the stirring and mixing time is 15 minutes to 30 minutes.

[0019] In an optional embodiment, after the solid-liquid separation to obtain the tantalum hydroxide filtrate, the process further comprises:

[0020] The tantalum hydroxide filtrate is subjected to pulping and fluorine washing treatment;

[0021] In an optional embodiment, the pulping and fluorine washing treatment comprises:

[0022] The tantalum hydroxide filtrate is washed with dilute ammonia water, and after solid-liquid separation, the tantalum hydroxide filtrate after pulping and fluorine washing is obtained;

[0023] In an optional embodiment, the washing is performed 3 to 5 times;

[0024] In an optional embodiment, the fluorine content in the tantalum hydroxide filtrate after pulping and fluorine washing is less than 0.5 g / L.

[0025] In an optional embodiment, the drying process comprises:

[0026] The tantalum hydroxide filtrate is dried in an oven;

[0027] In an optional embodiment, the drying temperature is 180°C;

[0028] In an optional embodiment, the temperature raising condition is: after the temperature is raised to a drying temperature of 180° C., the temperature is kept constant;

[0029] In an optional embodiment, the insulation time is 12 hours to 16 hours.

[0030] In an optional embodiment, the temperature of the calcination treatment is not less than 850°C.

[0031] In an optional embodiment, in the crushing and screening process, the screen fineness is not less than 60 mesh.

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

[0033] The preparation method of the small Fee's tantalum oxide provided by the present invention effectively simplifies the process flow and reduces energy consumption and production costs by neutralizing the industrial tantalum liquid containing Ta2O5 with concentrated ammonia water at room temperature. This method not only reduces the consumption of ammonia and reduces the cost of raw materials, but also reduces the introduction of impurities by omitting the dilution step, thereby improving the purity of the product and the stability of the particle size. In addition, since the neutralization process does not require high temperature, the accuracy of the equipment and the skill requirements of the operator are relatively low, which helps to reduce equipment costs and operating costs, while reducing potential impacts on the environment, making the entire preparation process more environmentally friendly. Overall, this preparation method shows significant beneficial effects in improving production efficiency, reducing costs, improving product quality and environmental sustainability. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0035] Figure 1 This is a schematic flow chart of the method for preparing the small Fee tantalum oxide in the embodiment of the present application;

[0036] Figure 2 This is a comparative bar chart of the Fisher particle sizes of the product particles prepared in the examples and comparative examples of the present application. DETAILED DESCRIPTION

[0037] The embodiments of the present invention will be described in detail below in conjunction with the examples, but it will be appreciated by those skilled in the art that the following examples are only used to illustrate the present invention and should not be considered as limiting the scope of the present invention. If no specific conditions are specified in the examples, the conditions are carried out according to normal conditions or the conditions recommended by the manufacturer. If the manufacturer of the reagents or instruments used is not specified, they are all conventional products that can be obtained commercially.

[0038] refer to Figure 1 In the embodiment of the present application, a method for preparing small Fee's tantalum oxide is provided, comprising:

[0039] Step S1, using concentrated ammonia water to neutralize industrial tantalum liquid containing Ta2O5 at room temperature, and after solid-liquid separation, obtain tantalum hydroxide filtrate.

[0040] As mentioned above, small Fee's tantalum oxide is a special tantalum oxide material, which is characterized by an average particle size of less than 0.8 microns. This ultra-fine particle size tantalum oxide has important application value in many fields due to its unique physical and chemical properties.

[0041] As mentioned above, concentrated ammonia water, also called ammonia solution or ammonia water, is a solution formed by dissolving ammonia (NH3) gas in water. Ammonia is a colorless gas with a pungent odor and is alkaline. When ammonia gas reacts with water, ammonia water is formed, and its chemical formula can be expressed as NH3·H2O. The concentration of concentrated ammonia water usually refers to the mass percentage of ammonia in water. The concentration of concentrated ammonia water used in industry is generally between 15% and 30%.

[0042] As mentioned above, the raw material targeted in this embodiment is industrial tantalum liquid, which refers to a solution containing tantalum obtained in the hydrometallurgical process of tantalum. This solution is usually derived from the leaching, dissolution or other chemical treatment process of tantalum ore, and its main component is tantalum compounds, including tantalum pentoxide (Ta2O5) in solution form. Industrial tantalum liquid is an intermediate product for preparing tantalum products such as tantalum metal, tantalum powder, and tantalum oxide.

[0043] The above steps are to react industrial tantalum liquid (containing Ta2O5) with concentrated ammonia water to neutralize the acidic components in the tantalum liquid, and generate tantalum hydroxide (Ta(OH)5) precipitate through the neutralization reaction.

[0044] It is carried out at room temperature without additional heating, saving energy. It avoids side reactions or tantalum losses that may be caused by high temperature. Specifically, concentrated ammonia water is gradually added to the industrial tantalum liquid containing Ta2O5, while stirring to ensure full reaction.

[0045] The Ta2O5 in the tantalum liquid reacts with ammonia water to form tantalum hydroxide precipitate, and the reaction formula can be:

[0046] Ta2O5+5NH3+5H2O→2Ta(OH)5+5NH4 + .

[0047] This step is to separate the tantalum hydroxide precipitate generated by the reaction from the mother liquor through filtration or other solid-liquid separation techniques to obtain a relatively pure tantalum hydroxide filter cake, thereby improving the purity of the product and laying the foundation for the subsequent washing and drying steps.

[0048] It should be noted that in the traditional hydrometallurgical process, the aging step is usually used to promote the maturation of the precipitate, that is, to improve the crystallinity and stability of the precipitate. This usually requires a period of standing to allow the precipitate crystals to grow and defects to be repaired. However, in the method for preparing the small Fee tantalum oxide of the present application, no aging step is required. The reason is that the process of neutralizing the industrial tantalum liquid with concentrated ammonia water is fast enough to promote the rapid formation of tantalum hydroxide (Ta(OH)5), thereby reducing the need for aging to promote the maturation of the precipitate. The use of concentrated ammonia water provides a more favorable environment, allowing the tantalum hydroxide precipitate to form rapidly and have good crystallinity, thereby reducing the need for an aging step.

[0049] In summary, in this embodiment, the aging step is omitted due to the special design and optimization of the method, as well as the consideration of improving production efficiency and reducing costs. One of the innovations of this method is that by omitting the aging step, a fast, efficient and environmentally friendly tantalum liquid neutralization process is achieved.

[0050] Step S2, subjecting the tantalum hydroxide filtrate to drying, calcining, crushing and screening in sequence to obtain small Feeble tantalum oxide.

[0051] In the above step, the separated tantalum hydroxide filter cake is dried to remove the moisture therein to obtain dry tantalum hydroxide.

[0052] The dried tantalum hydroxide is more convenient for storage and transportation, and is ready for the calcination process. Specifically, it can be dried using an oven, a spray dryer or other drying equipment.

[0053] Wherein, the reaction formula of the calcination reaction can be:

[0054] Ta(OH)5→Ta2O5+5H2O.

[0055] The above-mentioned crushing and screening process is to crush and screen the calcined tantalum oxide to obtain the required particle size distribution of the small Fee tantalum oxide. The particle size of the product is controlled to meet the needs of specific applications and improve the uniformity and consistency of the product.

[0056] In some embodiments, the concentration of Ta2O5 contained in the industrial tantalum liquid is 50 g / L to 80 g / L. For example, the concentration of Ta2O5 contained in the industrial tantalum liquid can be 50 g / L, 50 g / L, 50 g / L, 50 g / L, and so on.

[0057] It should be noted that the industrial tantalum liquid referred to in this embodiment refers to a raw tantalum liquid containing Ta2O5 at a specific concentration of 50g / L to 80g / L.

[0058] In some embodiments, the step S1, neutralizing the industrial tantalum liquid containing Ta2O5 at room temperature with concentrated ammonia water, and obtaining a tantalum hydroxide filtrate after solid-liquid separation, comprises:

[0059] Step S11, adding concentrated ammonia water to the industrial tantalum liquid and stirring and mixing, and performing a neutralization treatment at room temperature.

[0060] Step S12, after stopping adding the concentrated ammonia solution, continue stirring and mixing to obtain a mixed solution.

[0061] Step S13, performing solid-liquid separation on the mixed solution to obtain the tantalum hydroxide filtrate.

[0062] As discussed above, continued stirring during the neutralization process aids in the uniform distribution and growth of the tantalum hydroxide particles, reduces defects in the precipitate formation process, and thereby reduces the need for aging.

[0063] In some embodiments, the concentrated ammonia water is 18% to 20% ammonia water. For example, the concentrated ammonia water may be 18%, 19%, 20%, and so on.

[0064] In some embodiments, concentrated ammonia water is added to the industrial tantalum liquid and stirred to mix, and then a neutralization treatment step is performed at room temperature, and the pH of the neutralized industrial tantalum liquid is 8 to 10. For example, the pH may be 8, 9, 10, and the like.

[0065] In this embodiment, the pH of the neutralized industrial tantalum solution is limited to 8-10. This specific pH range has an important role and effect on the entire preparation process of small Fee tantalum oxide.

[0066] Under the condition of pH value of 8-10, Ta2O5 in industrial tantalum liquid reacts with concentrated ammonia water to form tantalum hydroxide (Ta(OH)5) precipitate. This pH range is conducive to the formation of tantalum hydroxide precipitate and can reduce the co-precipitation of impurity ions. At a specific pH value, the selectivity of the reaction can be improved, so that more Ta2O5 is converted into tantalum hydroxide precipitate, reducing unreacted Ta2O5 and other impurities.

[0067] In some embodiments, the stirring and mixing time is 15 minutes to 30 minutes. For example, the time can be 15 minutes, 18 minutes, 20 minutes, 22 minutes, 25 minutes, 28 minutes, 30 minutes, etc.

[0068] As mentioned above, by continuing to stir for 15 to 30 minutes after adding concentrated ammonia water, it is possible to ensure that the neutralization reaction is carried out evenly throughout the industrial tantalum liquid, avoid the generation of local over-reaction or unreacted areas, and promote the uniform formation of tantalum hydroxide precipitation. This specific stirring time helps to improve the efficiency of the neutralization reaction, ensure that the concentrated ammonia water fully reacts with the Ta2O5 in the industrial tantalum liquid, and control the physical properties of the tantalum hydroxide precipitate, such as particle size and morphology, which is crucial for the subsequent solid-liquid separation, drying, calcination and screening steps and the quality of the final product.

[0069] In some embodiments, after solid-liquid separation to obtain tantalum hydroxide filtrate, step S1 further comprises:

[0070] Step S3, subjecting the tantalum hydroxide filtrate to pulping and fluorine washing treatment.

[0071] As mentioned above, the pulping fluorine washing treatment is a specific step in the hydrometallurgical process, which is mainly used to remove fluoride ions in metal hydroxide precipitates (such as tantalum hydroxide).

[0072] In the process of preparing small Fee's tantalum oxide, the pulping and fluorine washing step is crucial because it can significantly improve the purity of small Fee's tantalum oxide products, thereby improving their electrical and chemical properties, which is essential to meet the needs of high-performance applications. In addition, fluorine impurities may affect the electrical and chemical properties of tantalum oxide, such as dielectric constant, conductivity, etc., and removing fluorine helps to maintain or improve these properties; in addition, the accumulation of fluoride ions in the environment may cause ecological problems, and reducing fluorine emissions through fluorine washing treatment will help protect the environment.

[0073] In some embodiments, the step S3, pulping and fluorine washing treatment, comprises:

[0074] Step S31, washing the tantalum hydroxide filtrate with dilute ammonia water, and obtaining the tantalum hydroxide filtrate after pulping and fluorine washing after solid-liquid separation.

[0075] In the above steps, the tantalum hydroxide filtrate is mixed with dilute ammonia water, and the fluoride ions are dissolved and removed by physical stirring. After washing, solid-liquid separation is performed again to separate the washing liquid and tantalum hydroxide.

[0076] Among them, in the pulping and fluorine washing process, the reaction formula can be:

[0077] Ta(OH)5·F - +NH3·H2O→Ta(OH)5+NH 4+ ·F - +H2O.

[0078] In some embodiments, the washing is performed 3 to 5 times; for example, the washing may be performed 3 times, 4 times, 5 times, and so on.

[0079] In some embodiments, the fluorine content in the tantalum hydroxide filtrate after pulping and fluorine washing is less than 0.5 g / L.

[0080] In some embodiments, the drying process comprises:

[0081] The tantalum hydroxide filtrate is dried in an oven;

[0082] In some embodiments, the drying temperature is 180°C;

[0083] In some embodiments, the temperature raising condition is: after the temperature is raised to a drying temperature of 180° C., the temperature is kept constant;

[0084] In some embodiments, the insulation time is 12 hours to 16 hours. For example, the insulation time can be 12 hours, 13 hours, 14 hours, 15 hours, 16 hours, etc.

[0085] In some embodiments, the calcination temperature is not less than 850°C.

[0086] In some embodiments, in the crushing and screening process, the screen fineness is not less than 60 mesh.

[0087] Example 1

[0088] In this embodiment, the preparation of small Fee's tantalum oxide was carried out for industrial tantalum liquid.

[0089] Experimental methods:

[0090] (1) 7000L of industrial tantalum liquid, with a tantalum oxide content of 50g / L, was neutralized at room temperature by adding 18% concentrated ammonia water, and the pH was adjusted to 9. Stirring was continued for 20 minutes without aging, and solid-liquid separation was performed to obtain a tantalum hydroxide filter cake.

[0091] (2) Pulping and fluorine washing treatment: The tantalum hydroxide filter cake is washed with diluted ammonia water at pH = 11 for 3 times. The fluorine content in the mother liquor is controlled at < 0.5 g / L. After solid-liquid separation, wet tantalum hydroxide is obtained.

[0092] (3) The wet tantalum hydroxide is placed in a drying oven to dry out the moisture, the drying temperature is set to 180° C., the temperature is raised to 180° C. and the temperature is kept at 12 hours to obtain dry tantalum hydroxide.

[0093] (4) Calcination and crushing: Calcine the dry tantalum hydroxide at 850°C, 45min;

[0094] The calcined tantalum oxide is crushed into fine powder, and after sieving, the -60 mesh undersize is obtained, namely, the small Fee tantalum oxide.

[0095] Example 2

[0096] In this embodiment, the preparation of small Fee's tantalum oxide was carried out for industrial tantalum liquid.

[0097] Experimental methods:

[0098] The method used in this embodiment is basically the same as that in Embodiment 1, except that:

[0099] (1) The tantalum oxide content in the industrial tantalum liquid is 55 g / L; the concentrated ammonia water is 19% ammonia water.

[0100] (2) Wash with dilute ammonia water 4 times;

[0101] (3) During drying, the temperature is raised to 180°C and kept warm for 14 hours.

[0102] Example 3

[0103] In this embodiment, the preparation of small Fee's tantalum oxide was carried out for industrial tantalum liquid.

[0104] Experimental methods:

[0105] The method used in this embodiment is basically the same as that in Embodiment 1, except that:

[0106] (1) The content of tantalum oxide in industrial tantalum liquid is 60g / L; concentrated ammonia water is 19% ammonia water. Stir for 25 minutes;

[0107] (2) Wash with dilute ammonia water 5 times;

[0108] (3) During drying, the temperature is raised to 180°C and kept warm for 16 hours. The calcined tantalum oxide is crushed into fine powder, and after sieving, the -60 mesh undersize is obtained, namely, the small Fee tantalum oxide.

[0109] Comparative Example 1

[0110] In this comparative example, the following method was used to prepare Fischer-Lehr tantalum oxide.

[0111] Experimental methods:

[0112] (1) 7000L of industrial tantalum liquid, with a tantalum oxide content of 55g / L, was neutralized at room temperature by adding liquid ammonia, the pH was adjusted to 9, and stirring was continued for 20 minutes without aging, and tantalum hydroxide filter cake was obtained by solid-liquid separation.

[0113] (2) Pulping and fluorine washing treatment: The tantalum hydroxide filter cake is washed with diluted ammonia water at pH = 11 for 3 times. The fluorine content in the mother liquor is controlled at < 0.5 g / L. After solid-liquid separation, wet tantalum hydroxide is obtained.

[0114] (3) The wet tantalum hydroxide is placed in a drying oven to dry out the moisture, the drying temperature is set to 180° C., the temperature is raised to 180° C. and then kept warm for 10 hours to obtain dry tantalum hydroxide.

[0115] (4) Calcination and crushing: Calcine the dry tantalum hydroxide at 850°C, 45min;

[0116] The calcined tantalum oxide is crushed into fine powder, and after sieving, the -60 mesh undersize is obtained, namely, the small Fee tantalum oxide.

[0117] Comparative Example 2

[0118] In this comparative example, the following method was used to prepare Fischer-Lehr tantalum oxide.

[0119] Experimental methods:

[0120] The method used in this embodiment is basically the same as that in Embodiment 2, except that:

[0121] Drying and heat preservation time 12h;

[0122] Comparative Example 3

[0123] In this comparative example, the following method was used to prepare Fischer-Lehr tantalum oxide.

[0124] Experimental methods:

[0125] The method used in this embodiment is basically the same as that in Embodiment 3, except that:

[0126] Add dilute ammonia water to wash twice;

[0127] Test results and analysis:

[0128] Test method:

[0129] The particle sizes of the products obtained in Examples 1 to 3 and Comparative Examples 1 to 3 were measured respectively using a laser particle size analyzer.

[0130] Test results:

[0131] Table 1. Fisher's particle size of the product particles prepared in the examples and comparative examples

[0132]

[0133] analyze:

[0134] (1) Refer to the data in Table 1 and Figure 2 It can be seen that the Fischer-Lehr particle sizes of the small Fischer-Lehr tantalum oxide prepared in Examples 1 to 3 were successfully controlled below 0.8 μm, indicating that the preparation method adopted can effectively prepare tantalum oxide with small particle size, and the method has good consistency and repeatability.

[0135] (2) In Examples 1 to 3, as the tantalum oxide content in the industrial tantalum liquid increases, the Fischer-Lehr particle size shows an upward trend. This is because the crystal growth rate exceeds the nucleation rate during the neutralization and crystallization process at a high content, resulting in the formation of tantalum oxide with a larger particle size.

[0136] (3) In Comparative Example 1, liquid ammonia was used for neutralization. Due to the high ammonia concentration, the solution volume changed little, and the fluorotantalate was not effectively diluted, which was not conducive to the formation of fine particles of tantalum oxide. This shows that the choice of neutralizer has a significant effect on the particle size of tantalum oxide.

[0137] (4) In Comparative Example 2, since the drying and holding time of tantalum hydroxide is only 12 hours, the moisture content in tantalum hydroxide is too high, and it is easy to agglomerate during the calcination process, which is not conducive to the formation of fine-particle tantalum oxide. This shows that the drying and holding time has an important influence on the particle size and quality of tantalum oxide.

[0138] (5) In Comparative Example 3, since only two washings with dilute ammonia water were performed, the fluorine in the tantalum hydroxide could not be completely removed, resulting in a high fluorine content in the tantalum oxide after calcination and a high loss on ignition value, making it impossible to produce qualified tantalum oxide. This shows that the number of washings has a direct impact on the purity and quality of tantalum oxide.

[0139] In summary, by comparing the results of different embodiments and comparative examples, the best operating conditions, such as tantalum oxide content, neutralizing agent selection, washing times, and drying and heat preservation time, can be explored to optimize the preparation process of small Fee's tantalum oxide. Among them, the results of comparative examples 1 to 3, compared with the embodiments, clearly show the superiority of the method used in the embodiments, especially in terms of particle size control and product quality, indicating that process parameters such as the selection of neutralizing agent, washing times, and drying and heat preservation time have a significant effect on the particle size and quality of the final product.

[0140] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein by equivalents. However, these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing small Fee's tantalum oxide, characterized in that: include: The industrial tantalum liquid containing Ta2O5 is neutralized at room temperature by concentrated ammonia water, and after solid-liquid separation, a tantalum hydroxide filtrate is obtained; The tantalum hydroxide filtrate is sequentially subjected to drying treatment, calcination treatment and crushing and screening treatment to obtain small Fee's tantalum oxide.

2. The method for preparing small Fee-shaped tantalum oxide as claimed in claim 1, characterized in that: The concentration of Ta2O5 contained in industrial tantalum liquid is 50g / L~80g / L.

3. The method for preparing small Fee-shaped tantalum oxide as claimed in claim 1, characterized in that: The industrial tantalum liquid containing Ta2O5 is neutralized at room temperature by concentrated ammonia water, and after solid-liquid separation, a tantalum hydroxide filtrate is obtained, which includes: Adding concentrated ammonia water to the industrial tantalum liquid and stirring and mixing, and performing a neutralization treatment at room temperature; After stopping adding the concentrated ammonia solution, continue stirring and mixing to obtain a mixed solution; The mixed liquid is subjected to solid-liquid separation to obtain the tantalum hydroxide filtrate.

4. The method for preparing small Fee-shaped tantalum oxide as claimed in claim 3, characterized in that: The concentrated ammonia water is 18% to 20% ammonia water.

5. The method for preparing small Fee-shaped tantalum oxide as claimed in claim 3, characterized in that: Concentrated ammonia water is added to the industrial tantalum liquid and stirred to mix, and then a neutralization treatment step is performed at room temperature. The pH value of the neutralized industrial tantalum liquid is 8-10.

6. The method for preparing small Fee-shaped tantalum oxide as claimed in claim 3, characterized in that: The stirring and mixing time is 15 minutes to 30 minutes.

7. The method for preparing small Fee-shaped tantalum oxide as claimed in claim 1, characterized in that: After the solid-liquid separation, after obtaining the tantalum hydroxide filtrate, the method further comprises: The tantalum hydroxide filtrate is subjected to pulping and fluorine washing treatment; Preferably, the pulping and fluorine washing treatment comprises: The tantalum hydroxide filtrate is washed with dilute ammonia water, and after solid-liquid separation, the tantalum hydroxide filtrate after pulping and fluorine washing is obtained; Preferably, the washing is performed 3 to 5 times; Preferably, the fluorine content in the tantalum hydroxide filtrate after pulping and fluorine washing is less than 0.5 g / L.

8. The method for preparing small Fee-shaped tantalum oxide as claimed in claim 1, characterized in that: The drying process comprises: The tantalum hydroxide filtrate is dried in an oven; Preferably, the drying temperature is 180°C; Preferably, the heating condition is: heating to a drying temperature of 180°C and then keeping warm; Preferably, the insulation time is 12 hours to 16 hours.

9. The method for preparing small Fee-shaped tantalum oxide as claimed in claim 1, characterized in that: The calcination temperature is not less than 850°C.

10. The method for preparing small Fee-shaped tantalum oxide according to claim 1, characterized in that: In the crushing and screening process, the screen fineness is not less than 60 meshes.

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