A method for producing tantalum powder using tantalum metallurgical by-products

Abstract

The application discloses a method for producing tantalum powder by using tantalum metallurgy by-products, and relates to the technical field of tantalum metallurgy, which comprises the following steps: uniformly mixing potassium fluotantalate and tantalum metallurgy by-products, loading the mixture into a reaction furnace, and adding sodium; heating the reaction furnace to 600-750 DEG C to make the potassium fluotantalate react with the sodium; adjusting the temperature in the furnace to 850-950 DEG C to perform sodium distillation after the reaction is completed, and introducing the sodium vapor into a condenser; adjusting the temperature in the reaction furnace to room temperature after the sodium distillation is completed, and taking out the reaction product; separating the tantalum powder and secondary by-products in the reaction product, and crushing and drying the separated secondary by-products to be used as the tantalum metallurgy by-products. The by-products generated in the tantalum metallurgy production process are used to remove residual sodium by distillation, clarification and separation, crushing and drying, and then directly used as a diluent for the reduction of potassium sodium fluotantalate, so that the melting point of the molten salt is reduced, and the energy-saving purpose is achieved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of tantalum metallurgy, and particularly relates to a method for producing tantalum powder by using tantalum metallurgy by-products. BACKGROUND

[0002] The potassium sodium fluorotantalate reduction method for preparing tantalum powder is a method for preparing tantalum powder by using potassium sodium fluorotantalate as a main raw material and using sodium chloride, potassium chloride, potassium fluoride and the like as a diluent. The main reaction mechanism is as follows:

[0003] K2TaF7+5Na=Ta+5NaF+2KF

[0004] The above reaction occurs between K2TaF7 and liquid sodium under the protection of argon and at a certain temperature. The reaction is an exothermic reaction, and a large amount of heat is released after the reaction starts, so that the reaction speed is too fast. Therefore, the reaction speed is controlled by heat absorption of the halide or halide mixture, and the halide does not participate in the chemical reaction in the whole reduction process. In the actual production process, the reduction process is controlled by controlling the temperature rising curve, which is the key link for controlling the performance of the tantalum powder. After the tantalum powder obtained is washed with water and acid and then is subjected to heat treatment, the final tantalum powder is obtained by magnesium reduction and deoxidization.

[0005] Therefore, the tantalum metallurgy by-products are a mixture of sodium fluoride, potassium fluoride and the original diluent halide, and the appearance is generally a purple porous block with a light blue and white inclusion and strong corrosion. The sodium reduction method for preparing tantalum powder uses one or more of sodium chloride, potassium chloride and potassium fluoride as a diluent, and uses metallic sodium to reduce potassium sodium fluorotantalate to obtain tantalum powder. The by-products are a molten salt mixture, and the main components are sodium chloride, potassium chloride, potassium fluoride and sodium fluoride, and the by-products contain recoverable superfine tantalum powder and trace amounts of oxides.

[0006] The traditional domestic treatment method is to concentrate the by-products in a large wastewater pool, dissolve the by-products by using wastewater generated in a later-stage tantalum powder purification process, extract superfine tantalum powder and oxides in filter residues, and send the tantalum powder to a wet extraction process for recovery. However, the wastewater contains a large amount of F - , Cl - ions, which are harmful to the environment and cannot be discharged at will. SUMMARY

[0007] In order to solve the above technical problems, the present application provides a method for producing tantalum powder by using tantalum metallurgy by-products, and the specific technical scheme is as follows.

[0008] The method for producing tantalum powder by using tantalum metallurgy by-products is that sodium chloride, potassium chloride and potassium fluoride are used as a diluent in the tantalum metallurgy, and potassium sodium fluorotantalate is reduced by sodium to prepare tantalum. The method comprises the following steps.

[0009] Step 1: uniformly mix potassium sodium fluorotantalate and tantalum metallurgy by-products, and then load the mixture into a reaction furnace and add sodium.

[0010] Step 2: heating the reaction furnace to 600-750℃ to react potassium fluorotantalate and sodium;

[0011] Step 3: adjusting the temperature in the furnace to 850-950℃ after the reaction to distill sodium, and introducing sodium vapor into the condenser tank;

[0012] Step 4: adjusting the temperature in the reaction furnace to room temperature after the sodium distillation to take out the reaction product;

[0013] Step 5: separating the tantalum powder and secondary by-products in the reaction product, and crushing and drying the separated secondary by-products to be used as the tantalum metallurgy by-products in Step 1.

[0014] Preferably, the separation method of the tantalum powder and secondary by-products in Step 5 is mechanical separation or manual separation; and the separated secondary by-products are crushed into solid blocks with a particle size of 40-55mm by a jaw crusher.

[0015] Preferably, the separated secondary by-products in Step 5 are dried in a F- and Cl- corrosion resistant vacuum oven, the drying temperature is 100-200℃, and the drying time is 5-30h.

[0016] Preferably, the water content of the dried secondary by-products in Step 5 is ≤0.05%.

[0017] Preferably, the mixing ratio of potassium fluorotantalate and tantalum metallurgy by-products in Step 1 is 1:(2-10).

[0018] Preferably, the reaction in Step 2 is carried out in an argon protective atmosphere or in an argon flowing atmosphere.

[0019] Preferably, the condenser tank in Step 3 is a three-stage condenser structure, which includes an upper condensing zone, a middle condensing zone and a lower condensing zone from top to bottom, the temperature of the upper condensing zone is 400-500℃, the temperature of the middle condensing zone is 300-400℃, and the temperature of the lower condensing zone is 100-150℃.

[0020] Preferably, the tantalum metallurgy by-products in Step 1 can also be mixed with a ceramic-conductive molecular composite catalyst, which is formed by compounding ceramic materials with conductive polymers or ceramic materials with metal oxides.

[0021] Preferably, the ceramic-conductive molecular composite catalyst is formed by compounding ceramic materials with conductive polymers, and the preparation process includes the following steps:

[0022] After calcining the aluminum oxide powder at 700-800℃, adding deionized water, and uniformly dispersing to obtain an aluminum oxide suspension;

[0023] Dissolving the pyrrole monomer and ammonium persulfate in a solvent to prepare the polypyrrole;

[0024] Adding the alumina suspension into the polypyrrole synthesis reaction solution, removing the excess solvent by stirring or ultrasonic treatment and filtering to obtain the polypyrrole-alumina composite material;

[0025] Drying the obtained composite material at 60-80℃ for 12h to remove the solvent;

[0026] Carrying out heat treatment on the composite material at 300-500℃ to obtain the product.

[0027] Preferably, the ceramic-conductive molecular composite catalyst is prepared by compounding the ceramic material with the metal oxide, and the preparation process comprises the following steps:

[0028] Carrying out calcination treatment on the alumina powder at 700-800℃;

[0029] Dissolving cerium nitrate in deionized water, and adding ammonia water to adjust the pH to 8-9;

[0030] Carrying out calcination at 600-700℃ for 4h after drying to obtain cerium oxide;

[0031] Mixing the cerium oxide and the calcined alumina powder uniformly according to the mass ratio of 1:1, adding deionized water to form a composite slurry, and uniformly dispersing by stirring or ultrasonic treatment;

[0032] Drying the composite slurry at 60-100℃ for 12h, and sintering at 800-1000℃ for 3-5h to obtain the product.

[0033] The method for producing tantalum powder from tantalum metallurgical by-products has the following beneficial effects:

[0034] 1. The by-products generated in the process of tantalum metallurgical production are directly used as diluents for the reduction of potassium sodium fluorotantalate after distillation, desalination, crushing, drying, which can reduce the melting point of the molten salt and achieve the purpose of energy saving.

[0035] 2. The composite salt contains superfine tantalum powder and tantalum oxide, which can effectively improve the direct recovery rate of tantalum powder.

[0036] 3. The method realizes the reuse of waste resources, reduces environmental pollution, and the produced tantalum powder meets the industry standard of metallurgical tantalum powder, which is environmentally friendly and saves production cost. DETAILED DESCRIPTION

[0037] In order for those skilled in the art to better understand the technical solutions of the present application, the present application will be described in detail below, and the description in this part is only exemplary and explanatory, and should not have any limiting effect on the protection scope of the present application.

[0038] The present embodiment provides a method for producing tantalum powder using tantalum metallurgy by-products, wherein at least one of sodium chloride, potassium chloride and potassium fluoride is used as a diluent for the reduction of potassium tantalate fluoride by sodium to produce tantalum, and the method comprises the following steps:

[0039] Step 1: uniformly mix potassium tantalate fluoride and tantalum metallurgy by-products, and then put them into a reaction furnace, and add sodium.

[0040] Step 2: heat the reaction furnace to 600-750°C to make the potassium tantalate fluoride and sodium react.

[0041] Step 3: after the reaction is completed, adjust the temperature in the furnace to 850-950°C to distill sodium, and introduce the sodium vapor into a condenser.

[0042] Step 4: after the sodium distillation is completed, adjust the temperature in the reaction furnace to room temperature, and take out the reaction product.

[0043] Step 5: separate the tantalum powder and secondary by-products in the reaction product, and after the separation, the secondary by-products are crushed and dried to be used as the tantalum metallurgy by-products in Step 1.

[0044] In the method for producing tantalum powder by reducing potassium tantalate fluoride with sodium, the by-products mainly include sodium fluoride and potassium fluoride. After the potassium tantalate fluoride and the tantalum metallurgy by-products are uniformly mixed, they are put into a reaction furnace, and sodium is added. At a temperature of 600-750°C, the sodium will react with the potassium tantalate fluoride. This reaction can reduce the tantalum in the potassium tantalate fluoride to tantalum metal. The sodium acts as a reducing agent in this process, separating the tantalum from the fluoride to form tantalum powder and sodium fluoride and potassium fluoride.

[0045] After the reduction reaction is completed, the furnace temperature is adjusted to 850-950°C to start the sodium distillation. The sodium distillation can evaporate the excess sodium to avoid its interference with the subsequent operation. The sodium vapor will evaporate from the furnace at high temperature and enter the condenser for condensation and recovery. The sodium distillation can effectively remove the excess sodium in the reaction, obtaining more pure tantalum powder.

[0046] After the distillation is completed, the furnace temperature is adjusted to 300-400°C, and the reaction product is taken out. At this time, the tantalum in the potassium tantalate fluoride has been reduced to a solidified block of metallic tantalum powder, and the sodium has been evaporated. The low temperature helps to control the tantalum extraction process and prevent further reaction of the tantalum powder and other substances. In Step 5, the tantalum powder is separated from the secondary by-products in the reaction product. The tantalum powder is usually separated by physical methods such as screening and sedimentation. After crushing and drying, the secondary by-products can be used as tantalum metallurgy by-products again in Step 1, realizing the recycling.

[0047] During the reaction of sodium reduction of potassium fluotantalate, sodium as a reducing agent can effectively reduce tantalum metal from potassium fluotantalate, and at the same time, excess sodium is removed by high-temperature distillation to obtain high-purity tantalum powder. Through step 5, the secondary by-product can be recycled for efficient use of resources.

[0048] The method for producing tantalum powder by using tantalum metallurgical by-products provided by the embodiment has the following beneficial effects:

[0049] 1. The by-product generated in the tantalum metallurgical production process is directly used as a diluent for the reduction of potassium fluotantalate sodium after distillation to remove residual sodium, clarification separation, crushing and drying, which can reduce the melting point of the molten salt and achieve the purpose of energy saving.

[0050] 2. The composite salt contains superfine tantalum powder and tantalum oxide, which can effectively improve the direct recovery rate of tantalum powder.

[0051] 3. The recycling of waste resources is realized, and environmental pollution is reduced. The produced tantalum powder meets the industry standard of metallurgical tantalum powder, which is environmentally friendly and saves production cost.

[0052] Further, the separation method of tantalum powder and secondary by-product in step 5 is mechanical separation or manual separation. The secondary by-product after separation is crushed into solid blocks with a particle size of 40-55mm by a jaw crusher.

[0053] Among them, the density of tantalum powder is larger, usually heavier than other by-products, so it can be separated from the secondary by-product by physical separation methods such as vibrating screen and air flow sorting. Manual separation can separate pure tantalum powder by manual screening and manual picking.

[0054] The separated secondary by-product is crushed by a jaw crusher to obtain solid blocks with a particle size of 40-55mm. These solid blocks will be used as raw materials for the next round of reaction and enter step 1, realizing the recycling of tantalum metallurgical by-products.

[0055] The crushed by-product usually needs to be dried. This is to remove the moisture or volatile substances in the by-product, so that the by-product is more suitable for entering the smelting process again.

[0056] Further, the secondary by-product after separation in step 5 is dried in a F - , Cl - corrosion-resistant vacuum oven, the drying temperature is 100-200℃, and the drying time is 5-30h.

[0057] The F-and Cl-corrosion resistant vacuum oven is a specially designed device that can resist the corrosion of fluorine ions (F-) and chlorine ions (Cl-). This is because fluorides and chlorides in tantalum metallurgy by-products have strong corrosive properties, and conventional ovens may not be able to withstand them.

[0058] The drying temperature range is set to 100-200℃. Within this temperature range, the moisture or volatile substances in the secondary by-products can be effectively removed without causing decomposition or deterioration of the tantalum or other components in the by-products.

[0059] The drying time is set to 5-30 hours, and the specific time is adjusted according to the water content and properties of the by-products. 5 hours is suitable for by-products with low moisture content or loose structure, and 30 hours is suitable for by-products with high moisture content or high density, and the drying process is relatively slow.

[0060] Further, the water content of the secondary by-products after drying in step 5 is ≤0.05%.

[0061] Further, the mixing ratio of potassium fluorotantalate and tantalum metallurgy by-products in step 1 is 1:(2-10), which can improve the utilization rate of reactants during the reaction and ensure that tantalum can be effectively extracted from the by-products. The amount of potassium fluorotantalate is less, while the amount of tantalum metallurgy by-products is more. More by-products can ensure that enough tantalum source participates in the reaction and provides enough raw materials for subsequent tantalum extraction.

[0062] The mixing ratio of the reactants directly affects the reduction efficiency of tantalum and the purity of tantalum powder. This ratio can optimize the reaction conditions, improve the extraction efficiency of tantalum, and maximize resource utilization during the reaction. During the implementation of the process, the specific ratio needs to be adjusted according to the properties of the by-products and the amount of potassium fluorotantalate.

[0063] Further, the reaction in step 2 is carried out under an argon protective atmosphere or in an argon flow atmosphere.

[0064] The argon protective atmosphere can effectively reduce the oxidation of sodium and tantalum and improve the selectivity and efficiency of the reduction reaction. The argon flow can promote the timely discharge of reaction gases and prevent gas accumulation from causing incomplete reactions or accumulation of by-products.

[0065] Further, the condenser tank in step 3 is a three-stage condenser structure, which includes an upper condensing zone, a middle condensing zone, and a lower condensing zone from top to bottom. The temperature of the upper condensing zone is 400-500℃, the temperature of the middle condensing zone is 300-400℃, and the temperature of the lower condensing zone is 100-150℃.

[0066] The third-stage condensing tower is usually a multi-stage segmented condensing system, which gradually reduces the temperature to condense the sodium vapor into liquid sodium in different temperature ranges and avoid mixing of the sodium vapor with other substances.

[0067] Further, the tantalum metallurgy by-product in step 1 can also be mixed with a ceramic-conductive molecular composite catalyst, which is formed by compounding a ceramic material with a conductive polymer or a ceramic material with a metal oxide.

[0068] The conductive polymer or metal oxide is compounded with the ceramic material to form the catalyst, and the ceramic material serves as a carrier of the catalyst, combining good thermal stability, chemical stability and a high specific surface area, and being compounded with a conductive or catalytically active polymer, metal oxide or metal nanoparticles, etc., to effectively improve the conductivity, catalytic activity and thermal stability of the catalyst. These composite materials can provide good catalytic performance in a high-temperature environment of sodium reduction of potassium fluotantalate and effectively accelerate the reduction reaction.

[0069] Further, the ceramic-conductive molecular composite catalyst is formed by compounding a ceramic material with a conductive polymer, and the preparation process thereof includes the following steps:

[0070] The alumina powder is calcined at 700-800°C and then added to deionized water, and after being uniformly dispersed, an alumina suspension is obtained.

[0071] The pyrrole monomer and ammonium persulfate are dissolved in a solvent to prepare a polypyrrole.

[0072] The alumina suspension is added to the synthesis reaction solution of the polypyrrole, and after stirring or ultrasonic treatment, the excess solvent is removed by filtration to obtain a composite material of polypyrrole loaded with alumina.

[0073] The obtained composite material is dried at 60-80°C for 12h to remove the solvent.

[0074] The composite material is heat treated at 300-500°C to obtain the ceramic-conductive molecular composite catalyst.

[0075] Further, the ceramic-conductive molecular composite catalyst is formed by compounding a ceramic material with a metal oxide, and the preparation process thereof includes the following steps:

[0076] The alumina powder is calcined at 700-800°C.

[0077] The cerium nitrate is dissolved in deionized water, and ammonia water is added to adjust the pH to 8-9.

[0078] After drying, the cerium oxide is prepared by calcining at 600-700°C for 4h.

[0079] The cerium oxide and the alumina powder after calcination are mixed uniformly in a mass ratio of 1:1, and then added into deionized water to form a composite slurry, which is uniformly dispersed by stirring or ultrasonic.

[0080] After the composite slurry is dried at 60-100℃ for 12h, it is sintered at 800-1000℃ for 3-5h to obtain the product.

[0081] The following provides specific examples, which can make those skilled in the art more fully understand the present application, but in no way limit the present application.

[0082] Example 1

[0083] Sodium chloride is used as a diluent, and potassium fluotantalate is used as a raw material to produce tantalum powder by liquid-liquid stirring sodium reduction process. After the sodium injection is completed, the reaction is carried out for 4h, residual sodium is removed by sodium distillation process, stirring is stopped and the temperature is kept constant for a certain time to ensure the separation of tantalum powder and by-products, and the tantalum powder and by-products are separated after cooling. The tantalum powder is crushed to small pieces with a particle diameter of about 50mm by using a crusher, and a F - , Cl - corrosion vacuum oven is used for drying at a temperature of 150℃ for 15h, and moisture is analyzed. 60kg of dried composite salt is weighed as a diluent, and tantalum powder is produced according to the requirements of the process of producing tantalum powder by sodium reduction of potassium fluotantalate. The results of the obtained tantalum powder are shown in Table 1.

[0084] Example 2

[0085] Potassium chloride is used as a diluent, and potassium fluotantalate is used as a raw material to produce tantalum powder by liquid-liquid stirring sodium reduction process. After the sodium injection is completed, the reaction is carried out for 4h, residual sodium is removed by sodium distillation process, stirring is stopped and the temperature is kept constant for a certain time to ensure the separation of tantalum powder and by-products, and the tantalum powder and by-products are separated after cooling. The tantalum powder is crushed to small pieces with a particle diameter of about 50mm by using a crusher, and a F - , Cl - corrosion vacuum oven is used for drying at a temperature of 150℃ for 15h, and moisture is analyzed. 60kg of dried composite salt is weighed as a diluent, and tantalum powder is produced according to the requirements of the process of producing tantalum powder by sodium reduction of potassium fluotantalate. The results of the obtained tantalum powder are shown in Table 1.

[0086] Example 3

[0087] Sodium chloride and potassium chloride are used as diluents, and potassium fluotantalate is used as a raw material to produce tantalum powder by liquid-liquid stirring sodium reduction process. After the sodium injection is completed, the reaction is carried out for 4h, residual sodium is removed by sodium distillation process, stirring is stopped and the temperature is kept constant for a certain time to ensure the separation of tantalum powder and by-products, and the tantalum powder and by-products are separated after cooling. The tantalum powder is crushed to small pieces with a particle diameter of about 50mm by using a crusher, and a F - , Cl -Corrosion vacuum oven, drying temperature is 150℃, time is 15 hours, moisture analysis. Weigh 60 kg of dried composite salt as diluent, according to the sodium reduction potassium fluorotantalate production process requirements of tantalum powder production, the results of tantalum powder see table 1.

[0088] Example 4

[0089] Potassium chloride, potassium fluoride as diluent potassium fluorotantalate as raw material, through the liquid-liquid stirring sodium reduction process production of tantalum powder, after the end of the injection of sodium by reaction 4h, sodium distillation process to remove residual sodium, stop stirring constant temperature for a certain time to ensure the separation of tantalum powder and by-product, after cooling tantalum powder and by-product separation, using the broken machine broken to the particle diameter of about 50mm small block, using drying equipment for F - , Cl - Corrosion vacuum oven, drying temperature is 150℃, time is 15 hours, moisture analysis. Weigh 60 kg of dried composite salt as diluent, according to the sodium reduction potassium fluorotantalate production process requirements of tantalum powder production, the results of tantalum powder see table 1.

[0090] Comparative example 1

[0091] The alumina powder is calcined at 800℃, then added to deionized water, and then added to polypyrrole. After ultrasonic treatment, filter and dry to obtain a ceramic-conductive molecular composite catalyst.

[0092] Sodium chloride as diluent, potassium fluorotantalate as raw material, and the prepared ceramic-conductive molecular composite catalyst is added. Through the liquid-liquid stirring sodium reduction process, tantalum powder is produced. After the end of the injection of sodium, the reaction time is 3h, which is shortened by 25%. The residual sodium is removed by sodium distillation process. Stop stirring and keep constant temperature for a certain time to ensure the separation of tantalum powder and by-product. After cooling, the tantalum powder and by-product are separated. The broken machine is broken to the particle diameter of about 50mm small block. The drying equipment is F-, Cl- corrosion vacuum oven, drying temperature is 150℃, time is 15 hours, moisture analysis. Weigh 60 kg of dried composite salt as diluent, according to the sodium reduction potassium fluorotantalate production process requirements of tantalum powder production, the results of tantalum powder see table 1.

[0093] Comparative example 2

[0094] The alumina powder is calcined at 800℃, then added to deionized water, and then added to polypyrrole. After ultrasonic treatment, filter and dry to obtain a ceramic-conductive molecular composite catalyst.

[0095] Sodium chloride is used as diluent, potassium fluotantalate is used as raw material, the prepared ceramic-conductive molecular composite catalyst is added, and the sodium reduction process is carried out through liquid-liquid stirring. After the sodium injection is completed, the reaction is carried out for 2.5 hours, and the reaction time is shortened by 37.5%. The residual sodium is removed through the sodium distillation process, the stirring is stopped, and the temperature is kept constant for a certain period of time to ensure that the tantalum powder and the by-product are layered. After cooling, the tantalum powder and the by-product are separated, and the tantalum powder is crushed to small pieces with a particle diameter of about 50mm using a crusher. A drying device that is resistant to F-and Cl-corrosion is used, the drying temperature is 150℃, the drying time is 15 hours, and the moisture content is analyzed. 60kg of the dried composite salt is weighed as a diluent, and the tantalum powder is produced according to the requirements of the sodium reduction potassium fluotantalate process. The results of the tantalum powder are shown in Table 1

[0096] Table 1: Analysis results of tantalum powder Unit: %

[0097]

[0098]

[0099] The principles and implementation modes of the present application are described by using specific examples in this paper, and the above examples are only used to help understand the method of the present application and its core idea. The above is only a preferred embodiment of the present application, but the protection scope of the present application is not limited to this. Any skilled person in the technical field can make equivalent replacement or change according to the technical scheme and the inventive concept of the present application within the technical range disclosed by the present application, which should be within the protection scope of the present application.

Claims

1. A method for producing tantalum powder from tantalum metallurgical by-products, characterized in that, The tantalum metallurgy adopts at least one of sodium chloride, potassium chloride and potassium fluoride as a diluent to prepare tantalum by reducing potassium fluotantalate with sodium, and the method comprises the following steps: S1: uniformly mixing potassium fluotantalate and a tantalum metallurgy by-product, loading into a reaction furnace, and adding sodium; S2: heating the reaction furnace to 600-750 DEG C, and reacting potassium fluotantalate and sodium; S3: after the reaction is completed, adjusting the temperature in the furnace to 850-950 DEG C to perform sodium distillation, and introducing sodium vapor into a condenser; S4: after the sodium distillation is completed, adjusting the temperature in the reaction furnace to room temperature, and taking out the reaction product; S5: separating tantalum powder and a secondary by-product in the reaction product, and using the separated secondary by-product after crushing and drying as the tantalum metallurgy by-product in step S1; In step S1, the tantalum metallurgy by-product is also mixed with a ceramic-conductive molecular composite catalyst, and the ceramic-conductive molecular composite catalyst is formed by compounding a ceramic material with a conductive polymer or a ceramic material with a metal oxide. The ceramic-conductive molecular composite catalyst is formed by compounding a ceramic material with a conductive polymer, and the preparation process comprises the following steps: Alumina powder is calcined at 700-800 DEG C, added into deionized water, uniformly dispersed to obtain an alumina suspension; Pyrrole monomers and ammonium persulfate are dissolved in a solvent to prepare polypyrrole; The alumina suspension is added into a synthesis reaction solution of polypyrrole, and after stirring or ultrasonic treatment, the excess solvent is removed by filtration to obtain a composite material of polypyrrole loaded with alumina; The obtained composite material is dried at 60-80 DEG C for 12 h to remove the solvent; After heat treatment of the composite material at 300-500 DEG C, the ceramic-conductive molecular composite catalyst is obtained. Or the ceramic-conductive molecular composite catalyst is formed by compounding a ceramic material with a metal oxide, and the preparation process comprises the following steps: Alumina powder is calcined at 700-800 DEG C; Cerium nitrate is dissolved in deionized water, and ammonia water is added to adjust the pH to 8-9; After drying, calcination is performed at 600-700 DEG C for 4 h to prepare cerium oxide; The cerium oxide and the calcined alumina powder are mixed uniformly at a mass ratio of 1:1, added into deionized water to form a composite slurry, and uniformly dispersed by stirring or ultrasonic treatment; After drying the composite slurry at 60-100 DEG C for 12 h, sintering is performed at 800-1000 DEG C for 3-5 h to obtain the ceramic-conductive molecular composite catalyst.

2. The method of claim 1, wherein, The separation method of the tantalum powder and the secondary by-product in step S5 is mechanical separation or manual separation; and the secondary by-product after separation is crushed into solid blocks with a particle size of 40-55 mm by a jaw crusher.

3. The method of claim 1, wherein, The separated secondary by-products in step S5 are dried in a corrosion-resistant vacuum oven at a temperature of 100-200°C for 5-30 hours. - , Cl - The dried product is then calcined in a muffle furnace at a temperature of 400-800°C for 1-10 hours.

4. The method of claim 1, wherein, The water content of the dried secondary by-product in step S5 is ≤0.05%.

5. The method of claim 1, wherein, The mixing ratio of potassium fluotantalate and the tantalum metallurgy by-product in step S1 is 1:(2-10).

6. The method of claim 1, wherein, The reaction in step S2 is performed in an argon protective atmosphere or in an argon flowing atmosphere.

7. The method of claim 1, wherein, The condensing tank in step S3 is a three-stage condensing tower structure, which comprises an upper condensing zone, a middle condensing zone and a lower condensing zone from top to bottom, the temperature of the upper condensing zone is 400-500 DEG C, the temperature of the middle condensing zone is 300-400 DEG C, and the temperature of the lower condensing zone is 100-150 DEG C.

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