CN108264088B - Method for preparing tantalum pentachloride from titanium-tantalum enriched slag - Google Patents
Method for preparing tantalum pentachloride from titanium-tantalum enriched slag Download PDFInfo
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Abstract
The invention provides a method for preparing tantalum pentachloride from titanium-tantalum enriched slag, which comprises the following steps: will contain Ta2O5The titanium-tantalum enriched slag and the carbon powder are uniformly mixed and put into a chlorination furnace for chlorineCarrying out a chemical reaction to generate mixed gas, and collecting the crystallized mixed gas into a dust collecting chamber at the temperature of 180-200 ℃ to obtain a crude product of tantalum pentachloride; and then placing the tantalum pentachloride crude product in a chlorination furnace, introducing chlorine gas to perform chlorination reaction, and collecting the crystallized tantalum pentachloride in the gas after the gas generated by the chlorination reaction passes through a dust collecting chamber with the temperature of 180-200 ℃. The titanium-tantalum-enriched slag is used as a raw material, the metal chloride obtained after chlorination of the enriched slag is used for realizing preparation of the tantalum pentachloride according to the boiling point difference of different metal chlorides, and the preparation method has the technical advantages of low raw material cost, high product added value, short flow and the like.
Description
Technical Field
The invention belongs to the technical field of non-ferrous metallurgy, and particularly relates to a method for preparing tantalum pentachloride from titanium-tantalum enriched slag.
Background
Tantalum pentachloride is white monoclinic crystal, can be decomposed even if trace moisture in the atmosphere, and is widely applied to the manufacture of capacitors, the preparation of high-temperature composite coatings and titanium alloy coatings, the preparation of aerogels and the like. The development of the process for preparing the tantalum pentachloride from the titanium tantalum enriched slag can bring considerable economic benefits to enterprises.
Tantalum is an important strategic reserve resource, and with the increasing exhaustion of mineral resources, the regeneration and cyclic utilization of secondary resources containing tantalum are carried out, so that the domestic demand pressure is effectively relieved. In recent years, with the rapid development of the aviation industry, thousands of tons of alloy waste materials are generated every year, and the comprehensive recovery of tantalum from tantalum-containing alloy waste materials has great market potential. The alloy waste is subjected to procedures of atomization powder spraying, sulfuric acid leaching, sodium salt roasting, water leaching and the like, nickel, cobalt, chromium, aluminum, tungsten, molybdenum and other elements are stripped, titanium-tantalum-enriched slag mainly containing titanium and tantalum is generated, wherein the titanium, tantalum, nickel, cobalt, chromium, tungsten, molybdenum and other metals mainly exist in a metal oxide state, and the titanium-tantalum-enriched slag is large in tantalum content and is a rare resource, so that the titanium-tantalum-enriched slag can be considered to be recycled. At present, no literature report related to treatment of the slag is available, so that the development of the tantalum pentachloride prepared from the titanium-tantalum-enriched slag has positive significance.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing tantalum pentachloride from titanium-tantalum enriched slag aiming at the defects of the prior art. The method adopts titanium-tantalum enriched slag as a raw material, realizes the preparation of the tantalum pentachloride by aiming at the boiling point difference of different metal chlorides, and has the technical advantages of low raw material cost, high product added value, short process and the like.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for preparing tantalum pentachloride from titanium-tantalum enriched slag is characterized by comprising the following steps:
step one, chlorination reaction: will contain Ta2O5Uniformly mixing the titanium-tantalum enriched slag and carbon powder, loading the mixture into a chlorination furnace, introducing argon into the chlorination furnace, replacing air in the chlorination furnace, continuously introducing chlorine into the chlorination furnace after the air is replaced, simultaneously raising the temperature in the chlorination furnace to 800-900 ℃, enabling the titanium-tantalum enriched slag to have chlorination reaction, generating mixed gas in the chlorination reaction process, enabling the mixed gas to pass through a dust collection chamber with the temperature of 180-200 ℃, and collecting the crystallized tantalum pentachloride in the mixed gas into the dust collection chamber to obtain a crude product of the tantalum pentachloride;
step two, secondary chlorination purification: placing the tantalum pentachloride crude product obtained in the step one in a chlorination furnace, introducing chlorine, raising the temperature in the chlorination furnace to 300-310 ℃, enabling gas generated after chlorination to pass through a dust collection chamber with the temperature of 180-200 ℃, and collecting crystallized tantalum pentachloride in the gas into the dust collection chamber to obtain tantalum pentachloride crystals with the mass purity not less than 99%.
The method for preparing tantalum pentachloride from titanium-tantalum enriched slag is characterized in that Ta in step one2O5The mass ratio of the carbon powder to the carbon powder is (5.5-6): 1.
the method for preparing the tantalum pentachloride from the titanium-tantalum enriched slag is characterized in that the flow rate of the chlorine gas in the step one is 1800 mL/min-2000 mL/min.
The method for preparing the tantalum pentachloride from the titanium-tantalum enriched slag is characterized in that the flow rate of the chlorine gas in the second step is 480 mL/min-500 mL/min.
The principle of preparing the tantalum pentachloride from the titanium-tantalum enriched slag comprises the following steps: the method of the invention utilizes tantalum and other impurity metals to produce metal chlorides after chlorination reaction, and the metal chlorides have different boiling points, and then obtains tantalum pentachloride crystals through gasification, condensation, separation and purification.
The chlorination reaction of the metal oxide in the titanium-tantalum-enriched slag comprises the following steps:
Ta2O5+5Cl2+2.5C＝2TaCl5+2.5CO2↑
TiO2+2Cl2+C＝TiCl4+CO2↑
SiO2+2Cl2+C＝SiCl4+CO2↑
2Fe2O3+6Cl2+C＝4FeCl3+3CO2↑。
TaCl generated by chlorination of titanium-tantalum enriched slag5、TiCl4、SiCl4And FeCl3The method comprises the steps of forming a mixed gas in a gaseous form, wherein the boiling point of titanium tetrachloride is 136.4 ℃, the boiling point of silicon tetrachloride is 57 ℃, the boiling point of ferric chloride is 315 ℃, the boiling point of tantalum pentachloride is 242 ℃, the chlorination temperature of primary chlorination is controlled to be 800-900 ℃, the temperature of a dust collection chamber is controlled to be 180-200 ℃, then crude tantalum pentachloride is deposited in the dust collection chamber, the titanium tetrachloride, the silicon tetrachloride and part of ferric chloride are discharged in a gaseous form through the dust collection chamber, and the crude tantalum pentachloride also contains part of crystallized ferric chloride; in the second step, the chlorination temperature is controlled to be 300-310 ℃ in the secondary chlorination, ferric chloride in the crude tantalum pentachloride does not reach the boiling point, so that the crude tantalum pentachloride is refined, and the tantalum pentachloride is collected by a dust collecting chamber again in a gas form, so that the separation of tantalum and impurities of titanium, iron and silicon is realized.
Compared with the prior art, the invention has the following advantages:
1. the invention takes titanium-tantalum-enriched slag obtained by pretreating alloy waste materials by a wet method as a raw material to prepare the tantalum pentachloride with higher purity, has the advantages of short flow, high added value and the like, provides a new idea for the preparation of the tantalum pentachloride, and avoids the environmental problem caused by adopting a hydrofluoric acid-extraction system.
2. The invention utilizes the characteristic that the boiling point numerical values of the tantalum and the impurity elements such as titanium, iron, silicon and the like have larger difference, so that the tantalum is separated and purified in the form of tantalum pentachloride. Wherein the boiling point of titanium tetrachloride is 136.4 ℃, the boiling point of silicon tetrachloride is 57 ℃, the boiling point of ferric chloride is 318 ℃, the boiling point of tantalum pentachloride is 242 ℃, the chlorination temperature is controlled to be 800-900 ℃ in the first chlorination, the temperature of the dust collection chamber is controlled to be 180-200 ℃, then the tantalum pentachloride and a small amount of iron are deposited in the dust collection chamber, and titanium, silicon and most of iron pass through the dust collection chamber in a gaseous form; the chlorination temperature of the secondary chlorination is controlled to be 300-310 ℃, and the refined tantalum pentachloride is collected by a dust collecting chamber in a gas form, so that the separation of tantalum and impurities of titanium, iron and silicon is realized.
The technical solution of the present invention will be described in further detail by examples.
Detailed Description
Example 1
The method of the embodiment comprises the following steps:
step one, chlorination reaction: weighing 1000g of titanium-tantalum enrichment slag, wherein the titanium-tantalum enrichment slag comprises the following main metal components in percentage by mass: 27% of Ta, 18% of Ti, 0.80% of Fe, 1.2% of Cr and 0.66% of Ni, wherein Ta in the titanium-tantalum enrichment slag is Ta2O5In the form of (1), other metals are also in the form of oxides, 1000g of titanium-tantalum-enriched slag and carbon powder are uniformly mixed and charged into a chlorination furnace, wherein Ta2O5And the mass ratio of the carbon powder to the carbon powder is 5.8: 1, introducing argon into the chlorination furnace, replacing air in the chlorination furnace, continuously introducing chlorine gas with the flow rate of 2000mL/min into the chlorination furnace after the air is replaced, simultaneously raising the temperature in the chlorination furnace to 850 ℃ to enable titanium-tantalum enriched slag to have chlorination reaction, generating mixed gas in the chlorination reaction process, enabling the mixed gas to pass through a dust collection chamber with the temperature of 170 ℃, and collecting the tantalum pentachloride crystals in the mixed gas into the dust collection chamber to obtain the pentachlorideDissolving a tantalum crude product;
the main reaction formula of the titanium-tantalum enriched slag in the first step is as follows:
Ta2O5+5Cl2+2.5C＝2TaCl5+2.5CO2↑
TiO2+2Cl2+C＝TiCl4+CO2↑
2Fe2O3+6Cl2+C＝4FeCl3+3CO2↑
Cr2O3+6Cl2+C＝4CrCl3+3CO2↑
NiO+6Cl2+C＝4NiCl2+3CO2↑。
wherein in the step one, TaCl is added when the reaction temperature is 850 DEG C5(boiling point 242 ℃ C.), TiCl4(boiling point 136.4 ℃ C.) and FeCl3(boiling point: 315 ℃ C.) is gaseous, CrCl3(boiling point 1500 ℃ C.) and NiCl2(boiling point 987 ℃) does not reach the boiling point, the mixture is still solid, and the mixed gas also contains products of carbon and oxygen, namely CO and CO2And Cl that does not participate in the chlorination reaction2Etc. but when the mixed gas passes through a dust collecting chamber at 180 deg.C, TiCl in the mixed gas4、CO、CO2、Cl2Is still in the gaseous state and TaCl is discharged5And FeCl3Forming crude tantalum pentachloride crystals in a crystallized dust collection chamber;
step two, secondary chlorination purification: placing the tantalum pentachloride crude product obtained in the step one in a chlorination furnace, introducing chlorine gas with the flow rate of 500mL/min, and raising the temperature in the chlorination furnace to 305 ℃, wherein the temperature does not reach FeCl3Thus TaCl5And the chlorine gas passes through the dust collection chamber at the temperature of 180 ℃ again, and the chlorine gas is discharged, so that tantalum pentachloride crystals with the mass purity of 99.5% are collected in the dust collection chamber, the mass of the tantalum pentachloride crystals is 482g, and the recovery rate of tantalum in the titanium-tantalum enriched slag is calculated to be 90.3%.
Example 2
The method of the embodiment comprises the following steps:
step one, chlorination reaction: weighing 1000g of titanium-tantalum enrichment slag, wherein the titanium-tantalum enrichment slag comprises the following main metal components in percentage by mass: 25% of Ta, 22% of Ti, 0.90% of Fe, 0.6% of Al, 1.1% of Cr and 0.7% of Ni, wherein Ta in the titanium-tantalum enrichment slag is Ta2O5The method comprises the steps of uniformly mixing 1000g of titanium-tantalum enriched slag and carbon powder, and filling the mixture into a chlorination furnace, wherein Ta in the titanium-tantalum enriched slag2O5And the mass ratio of the carbon powder to the carbon powder is 5.5: 1, introducing argon into the chlorination furnace, replacing air in the chlorination furnace, continuously introducing chlorine gas with the flow rate of 2000mL/min into the chlorination furnace after the air is replaced, simultaneously raising the temperature in the chlorination furnace to 800 ℃ to enable titanium-tantalum enriched slag to perform chlorination reaction, and generating mixed gas in the chlorination reaction process, wherein the mixed gas mainly comprises TaCl5、TiCl4、FeCl3、AlCl3、CO、CO2、Cl2The mixed gas passes through a dust collection chamber with the temperature of 190 ℃, wherein the tantalum pentachloride crystals in the mixed gas are collected into the dust collection chamber to obtain a crude product of the tantalum pentachloride;
the main reaction formula of the titanium-tantalum enriched slag in the first step is as follows:
Ta2O5+5Cl2+2.5C＝2TaCl5+2.5CO2↑
TiO2+2Cl2+C＝TiCl4+CO2↑
2Fe2O3+6Cl2+C＝4FeCl3+3CO2↑
2Al2O3+6Cl2+C＝4AlCl3+3CO2↑
Cr2O3+6Cl2+C＝4CrCl3+3CO2↑
NiO+6Cl2+C＝4NiCl2+3CO2↑。
wherein in the step one, TaCl is added when the reaction temperature is 850 DEG C5(boiling point 242 ℃ C.), AlCl3(boiling point 181 ℃ C.), TiCl4(boiling point 136.4 ℃ C.) and FeCl3(boiling point: 315 ℃ C.) is gaseous, CrCl3(boiling point 1500 ℃ C.) and NiCl2(boiling point 987 ℃) does not reach the boiling point, the mixture is still solid, and the mixed gas also contains products of carbon and oxygen, namely CO and CO2And Cl that does not participate in the chlorination reaction2Etc. but when the mixed gas passes through a dust collecting chamber at 190 deg.C, TiCl in the mixed gas4、AlCl3、CO、CO2And Cl2Is still in the gaseous state and TaCl is discharged5And FeCl3Forming crude tantalum pentachloride crystals in a crystallized dust collection chamber;
step two, secondary chlorination purification: placing the tantalum pentachloride crude product obtained in the step one in a chlorination furnace, introducing chlorine gas with the flow rate of 500mL/min, and raising the temperature in the chlorination furnace to 300 ℃, wherein the temperature does not reach FeCl3Thus TaCl5And passing through a dust collection chamber with the temperature of 190 ℃ again along with the chlorine gas, discharging the chlorine gas, collecting tantalum pentachloride crystals with the mass purity of 99.3% in the dust collection chamber, wherein the mass of the tantalum pentachloride crystals is 451g, and the recovery rate of tantalum in the titanium-tantalum enriched slag is 91.2% by calculation.
Example 3
The method of the embodiment comprises the following steps:
step one, chlorination reaction: weighing 1000g of titanium-tantalum enrichment slag, wherein the titanium-tantalum enrichment slag comprises the following main metal components in percentage by mass: 28% of Ta, 22% of Ti, 1.0% of Fe, 1.2% of Al, 0.7% of Cr and 0.8% of Ni, wherein Ta in the titanium-tantalum enrichment slag is Ta2O5The method comprises the steps of uniformly mixing 1000g of titanium-tantalum enriched slag and carbon powder, and filling the mixture into a chlorination furnace, wherein Ta in the titanium-tantalum enriched slag2O5And carbon powder in a mass ratio of 6: 1, introducing argon into the chlorination furnace, replacing air in the chlorination furnace, continuously introducing chlorine gas with the flow rate of 2000mL/min into the chlorination furnace after the air is replaced, simultaneously raising the temperature in the chlorination furnace to 900 ℃ to enable titanium-tantalum enriched slag to perform chlorination reaction, and generating mixed gas in the chlorination reaction process, wherein the mixed gas mainly comprises TaCl5、TiCl4、FeCl3、AlCl3、CO、CO2、Cl2HCl, the mixed gas passes throughA dust collection chamber with the temperature of 200 ℃, wherein tantalum pentachloride crystals in the mixed gas are collected into the dust collection chamber to obtain a crude product of tantalum pentachloride and a crude product of tantalum pentachloride;
the main reaction formula of the titanium-tantalum enriched slag in the first step is as follows:
Ta2O5+5Cl2+2.5C＝2TaCl5+2.5CO2↑
TiO2+2Cl2+C＝TiCl4+CO2↑
2Fe2O3+6Cl2+C＝4FeCl3+3CO2↑
2Al2O3+6Cl2+C＝4AlCl3+3CO2↑
Cr2O3+6Cl2+C＝4CrCl3+3CO2↑
NiO+6Cl2+C＝4NiCl2+3CO2↑。
wherein in the step one, TaCl is added when the reaction temperature is 850 DEG C5(boiling point 242 ℃ C.), AlCl3(boiling point 181 ℃ C.), TiCl4(boiling point 136.4 ℃ C.) and FeCl3(boiling point: 315 ℃ C.) is gaseous, CrCl3(boiling point 1500 ℃ C.) and NiCl2(boiling point 987 ℃) does not reach the boiling point, the mixture is still solid, and the mixed gas also contains products of carbon and oxygen, namely CO and CO2And Cl that does not participate in the chlorination reaction2Etc. but when the mixed gas passes through a dust collecting chamber at 200 deg.C, TiCl in the mixed gas4、AlCl3、CO、CO2And Cl2Is still in the gaseous state and TaCl is discharged5And FeCl3Forming crude tantalum pentachloride crystals in a crystallized dust collection chamber;
step two, secondary chlorination purification: placing the tantalum pentachloride crude product obtained in the step one in a chlorination furnace, introducing chlorine gas with the flow rate of 500mL/min, and raising the temperature in the chlorination furnace to 310 ℃, wherein the temperature does not reach FeCl3Thus TaCl5The chlorine gas passes through a dust collection chamber with the temperature of 200 ℃ again, the chlorine gas is discharged, and the quality collected in the dust collection chamberThe recovery rate of tantalum in the titanium tantalum enrichment slag is calculated to be 97.1 percent, wherein the mass of the tantalum pentachloride crystal is 504g, and the recovery rate of tantalum in the titanium tantalum enrichment slag is 99.4 percent.
Example 4
The method of the embodiment comprises the following steps:
step one, chlorination reaction: weighing 1000g of titanium-tantalum enrichment slag, wherein the titanium-tantalum enrichment slag comprises the following main metal components in percentage by mass: ta 28%, Ti 20%, Fe 1.10% and Si 4%, wherein Ta in the titanium-tantalum enrichment slag is Ta2O5The method comprises the steps of uniformly mixing 1000g of titanium-tantalum enriched slag and carbon powder, and filling the mixture into a chlorination furnace, wherein Ta in the titanium-tantalum enriched slag2O5And the mass ratio of the carbon powder to the carbon powder is 5.8: 1, introducing argon into the chlorination furnace, replacing air in the chlorination furnace, continuously introducing chlorine gas with the flow rate of 2000mL/min into the chlorination furnace after the air is replaced, simultaneously raising the temperature in the chlorination furnace to 850 ℃ to enable titanium-tantalum enriched slag to perform chlorination reaction, and generating mixed gas in the chlorination reaction process, wherein the mixed gas mainly comprises TaCl5、TiCl4、FeCl3、CO、CO2、Cl2The mixed gas passes through a dust collection chamber with the temperature of 170 ℃, wherein the tantalum pentachloride crystal in the mixed gas is collected into the dust collection chamber to obtain a crude product of the tantalum pentachloride;
the main reaction formula of the titanium-tantalum enriched slag in the first step is as follows:
Ta2O5+5Cl2+2.5C＝2TaCl5+2.5CO2↑
TiO2+2Cl2+C＝TiCl4+CO2↑
SiO2+2Cl2+C＝SiCl4+CO2↑
2Fe2O3+6Cl2+C＝4FeCl3+3CO2↑。
wherein in the step one, TaCl is added when the reaction temperature is 850 DEG C5(boiling point 242 ℃ C.), TiCl4(boiling point 136.4 ℃ C.) and FeCl3The boiling point is 315 ℃ and the gas is gaseous and does not reach the boiling point,the mixed gas still is solid, and the mixed gas also contains CO and CO products of carbon and oxygen2And Cl that does not participate in the chlorination reaction2Etc. but when the mixed gas passes through a dust collecting chamber at 200 deg.C, TiCl in the mixed gas4、AlCl3、CO、CO2And Cl2Is still in the gaseous state and TaCl is discharged5And FeCl3Forming crude tantalum pentachloride crystals in a crystallized dust collection chamber;
step two, secondary chlorination purification: and (2) placing the tantalum pentachloride crude product obtained in the step one in a chlorination furnace, introducing chlorine gas with the flow rate of 500mL/min, raising the temperature in the chlorination furnace to 305 ℃, enabling the gas obtained after chlorination to pass through a dust collection chamber with the temperature of 190 ℃, and collecting tantalum pentachloride crystals with the mass purity of 99.5% in the dust collection chamber, wherein the mass of the tantalum pentachloride crystals is 482g, and the recovery rate of tantalum in the titanium-tantalum enrichment slag is calculated to be 90.3%.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (3)
1. A method for preparing tantalum pentachloride from titanium-tantalum enriched slag is characterized by comprising the following steps:
step one, chlorination reaction: will contain Ta2O5Uniformly mixing the titanium-tantalum enriched slag and carbon powder, loading the mixture into a chlorination furnace, introducing argon into the chlorination furnace, replacing air in the chlorination furnace, continuously introducing chlorine into the chlorination furnace after the air is replaced, simultaneously raising the temperature in the chlorination furnace to 850-900 ℃, enabling the titanium-tantalum enriched slag to have chlorination reaction, generating mixed gas in the chlorination reaction process, enabling the mixed gas to pass through a dust collection chamber with the temperature of 180-200 ℃, and collecting the crystallized tantalum pentachloride in the mixed gas into the dust collection chamber to obtain a crude product of the tantalum pentachloride; said Ta2O5The mass ratio of the carbon powder to the carbon powder is (5.5-6): 1;
step two, secondary chlorination purification: and (2) placing the tantalum pentachloride crude product obtained in the step one in a chlorination furnace, introducing chlorine, raising the temperature in the chlorination furnace to 300-310 ℃, enabling gas generated after chlorination to pass through a dust collection chamber with the temperature of 180-200 ℃, and collecting crystallized tantalum pentachloride in the gas into the dust collection chamber to obtain tantalum pentachloride crystals with the mass purity not less than 99%.
2. The method for preparing tantalum pentachloride from titanium tantalum enriched slag according to claim 1, wherein the flow rate of the chlorine gas in the step one is 1800mL/min to 2000 mL/min.
3. The method for preparing tantalum pentachloride from titanium-tantalum enriched slag according to claim 1, wherein the flow rate of the chlorine gas in the second step is 480 mL/min-500 mL/min.
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