CN110563038A - method for preparing low-antimony low-iron high-purity niobium oxide from niobium tantalite - Google Patents
method for preparing low-antimony low-iron high-purity niobium oxide from niobium tantalite Download PDFInfo
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Abstract
a method for preparing low-antimony low-iron niobium oxide from niobium tantalite, comprising the steps of: (1) grinding niobium-tantalum-iron ore by an ore grinder, and then decomposing by acid; (2) after adjusting the acid, the decomposition liquid is extracted by an organic solvent, and metal ions such as tantalum, niobium, antimony, iron and the like enter an organic phase; (3) removing impurities of an organic phase of fluoroniobate or fluorotantalic acid containing metal ions such as antimony, iron and the like by using a pickling agent to obtain a tantalum-containing niobate washing organic phase; (4) performing two-stage niobium removal on the tantalum-containing niobate washing organic matter obtained in the step (3) by using a niobium removal agent to obtain two-stage niobium solution; (5) and (4) respectively introducing ammonia into the two sections of niobium liquid obtained in the step (4) for mixing, carrying out neutralization reaction to generate niobium hydroxide precipitate, and sequentially filtering, washing, drying and calcining to obtain the low-antimony low-iron niobium oxide and the high-antimony high-iron niobium oxide. The method can produce the low-antimony low-iron high-purity niobium oxide by utilizing the niobium-tantalum-iron ore, is simple to operate and is easy for industrial production.
Description
Technical Field
The invention relates to a method for preparing low-antimony low-iron high-purity niobium oxide from niobium-tantalum-iron ore.
Background
The high-purity niobium oxide is required to have low impurity content, especially impurity elements such as Fe, Cr and Sb, so that the raw materials are required to be high for producing the high-purity niobium oxide. The raw materials of tantalum-niobium products, namely tantalum-niobium ores, belong to scarce and non-renewable resources, and the grade of the tantalum-niobium raw materials is gradually reduced along with the continuous increase of the mining amount, so that antimony-containing tantalum-niobium raw materials are more and more. Compared with niobium concentrate, niobium-tantalum-iron ore has high content of impurities such as iron, antimony and the like, and antimony has similar properties to tantalum and niobium, so that antimony and niobium (tantalum) are difficult to be effectively separated in a general tantalum-niobium wet smelting process, and therefore, the niobium product or the tantalum product prepared by adopting the existing process has high antimony content, and the demand of the electronic industry and the metallurgical industry on high-quality tantalum-niobium products cannot be met.
Patent US005908489A discloses a method for removing antimony from a tantalum-niobium ore decomposition liquid, which adopts alkali metals such as Fe, Al and the like to reduce Sb in the tantalum-niobium ore decomposition liquid into a metallic state and remove Sb before extraction; CN108862384A discloses an antimony removal method, which comprises the steps of firstly converting positive pentavalent antimony in an antimony-containing niobium solution or an antimony-containing tantalum solution into positive trivalent antimony through a reduction reaction, then reacting the positive pentavalent antimony with a complexing agent to generate a stable antimony complex, and then precipitating niobium or tantalum in the solution to generate niobium hydroxide or tantalum hydroxide by utilizing a neutralization reaction, wherein the antimony complex is not damaged and exists in the solution, so that the high-efficiency separation of a niobium product or a tantalum product and antimony is realized; CN 109097572A discloses a method for removing impurity antimony in tantalum-niobium wet smelting, which comprises the steps of adding a water-soluble chemical complexing agent into a water solution of fluoroniobic acid or fluorotantalic acid containing antimony impurity metal ions, fully mixing, introducing ammonia into the mixed solution for neutralization to generate niobium hydroxide or tantalum hydroxide precipitate, filtering the precipitate, and washing with pure warm water to remove the antimony impurity metal ions coexisting in the precipitate. The method has the problems that complicated and harsh procedures need to be added, and the like, so that the popularization and the application of the technologies are restricted.
disclosure of Invention
The invention aims to provide a method for preparing low-antimony low-iron high-purity niobium oxide from niobium-tantalum-iron ore, solves the problem that the popularization and application of the technologies are restricted due to the fact that complicated and harsh working procedures need to be added in the existing method, and has the characteristics of simple process flow, simplicity and convenience in operation and suitability for industrial production.
The technical scheme adopted for achieving the aim is that the method for preparing the low-antimony low-iron high-purity niobium oxide from the niobium-tantalum-iron ore comprises the following steps:
(1) grinding niobium-tantalum-iron ore by an ore grinder, and then decomposing by acid;
(2) after adjusting the acid, the decomposition liquid is extracted by an organic solvent, and metal ions such as tantalum, niobium, antimony, iron and the like enter an organic phase;
(3) removing impurities of an organic phase of fluoroniobate or fluorotantalic acid containing metal ions such as antimony, iron and the like by using a pickling agent to obtain a tantalum-containing niobate washing organic phase;
(4) performing two-stage niobium removal on the tantalum-containing niobate washing organic matter obtained in the step (3) by using a niobium removal agent to obtain two-stage niobium solution;
(5) and (4) respectively introducing ammonia into the two sections of niobium liquid obtained in the step (4) for mixing, carrying out neutralization reaction to generate niobium hydroxide precipitate, and sequentially filtering, washing, drying and calcining to obtain the low-antimony low-iron niobium oxide and the high-antimony high-iron niobium oxide.
Advantageous effects
Compared with the prior art, the invention has the following advantages.
The preparation method has the advantages that the niobium oxide with low antimony and low iron content can be prepared by utilizing the niobium-tantalum-iron ore, so that the content of antimony in the niobium oxide is not higher than 10ppm, and the content of iron in the niobium oxide is not higher than 5ppm, and the preparation method has the characteristics of simple process flow, simplicity and convenience in operation and suitability for industrial production.
Detailed Description
A method for preparing low-antimony low-iron high-purity niobium oxide from niobium tantalite comprises the following steps:
(1) Grinding niobium-tantalum-iron ore by an ore grinder, and then decomposing by acid;
(2) After adjusting the acid, the decomposition liquid is extracted by an organic solvent, and metal ions such as tantalum, niobium, antimony, iron and the like enter an organic phase;
(3) Removing impurities of an organic phase of fluoroniobate or fluorotantalic acid containing metal ions such as antimony, iron and the like by using a pickling agent to obtain a tantalum-containing niobate washing organic phase;
(4) Performing two-stage niobium removal on the tantalum-containing niobate washing organic matter obtained in the step (3) by using a niobium removal agent to obtain two-stage niobium solution;
(5) and (4) respectively introducing ammonia into the two sections of niobium liquid obtained in the step (4) for mixing, carrying out neutralization reaction to generate niobium hydroxide precipitate, and sequentially filtering, washing, drying and calcining to obtain the low-antimony low-iron niobium oxide and the high-antimony high-iron niobium oxide.
The acid used for acid decomposition in the step (1) is one or two of hydrofluoric acid and sulfuric acid.
The organic solvent used for extraction in the step (2) is sec-octanol or methyl isobutyl ketone.
The pickling agent for pickling in the step (3) is a sulfuric acid solution with the concentration of 3.5-3.9 mol/L.
The niobium resisting agent in the step (4) adopts inorganic acid which is one or two of hydrofluoric acid and sulfuric acid, and preferably sulfuric acid; the two-stage niobium is H-containing in the first stage+One or two of hydrofluoric acid and sulfuric acid of 3-5mol/L are used as anti-niobium agent, and H is preferably contained+4.2mol/L dilute sulfuric acid, and the second stage adopts H-containing+2.8-3.3mol/L of hydrofluoric acid or sulfuric acid or both are used as anti-niobium agent, and H is preferably contained+3mol/L dilute sulfuric acid.
The form of the introduced ammonia in the step (5) is one of ammonia water, ammonia gas and liquid ammonia; the purity of the high-purity niobium oxide is more than or equal to 99.99 percent.
the present invention will be described in detail below with reference to specific examples.
The present invention was practiced using niotalcite having the composition shown in table 1.
Table 1 niobium tantalite chemical composition:
| item | Ta2O5 | Nb2O5 | Fe | Sb | W | Si | U3O2 | ThO2 |
| Mass content | 5.21 | 42.14 | 29.18 | 0.23 | 0.07 | 10.22 | 0.07 | 0.03 |
Example one
(1) 1000kg of niobium-tantalum-iron ore crushed to 300 meshes is treated with hydrofluoric acid and sulfuric acid according to a solid-to-liquid ratio of 1: (1.6-1.8): (0.5-0.6) carrying out acid leaching, and carrying out heat preservation reaction for 8 hours after acid is added, wherein the mass concentration of hydrofluoric acid is 55%, the mass concentration of sulfuric acid is 98%, and acid leaching liquid is obtained;
(2) Adjusting the acidity of the acid leaching solution to HF 6.8-7.0 mol/L by using hydrofluoric acid and sulfuric acid, and adjusting the pH to H2SO43.8-3.9 mol/L, using sec-octanol as extractant in 10-grade extraction tankCarrying out countercurrent extraction, wherein the volume ratio of the organic phase to the water phase is 1.2:1, so as to obtain an organic phase containing tantalum and niobium;
(3) Preparing a pickling agent with the concentration of 3.6 mol/L by using 98% CP pure sulfuric acid, wherein the volume ratio of the tantalum-niobium-containing organic phase to the pickling agent is 2.5:1, and carrying out 10-stage countercurrent washing to obtain an acid-washed organic phase;
(4) Preparing 3.8mol/L and 3mol/L sulfuric acid solutions by using 98% CP pure sulfuric acid as niobium-removing agents of the first-stage niobium-removing agent and the second-stage niobium-removing agent respectively, and extracting tantalum through the first-stage 15-grade niobium-removing agent, the second-stage 10-grade niobium-removing agent and the 10-grade tantalum-removing agent to obtain a first-stage niobium solution and a second-stage niobium solution;
(5) And (3) respectively introducing ammonia gas into the two sections of niobium-containing solutions to neutralize the solutions until the pH value is 9, and washing, drying and calcining the solutions by pure water to obtain a high-purity niobium oxide product and a common niobium oxide product.
through detection, the main component Nb of the product in the high-purity niobium oxide2O599.992 percent, 4.1ppm of impurity tantalum, 2.6ppm of ferrum and 5.8ppm of stibium, and other impurities can all meet the non-ferrous metal industry standard FNb2O5The requirement of 04 grades, the specific element components are shown in Table 2, the mass of the high-purity niobium oxide product is 290kg, the mass of the common niobium oxide product is 128kg, and the mass ratio is 2.27: 1.
Example two
(1) 1000kg of niobium-tantalum-iron ore crushed to 300 meshes is treated with hydrofluoric acid and sulfuric acid according to a solid-to-liquid ratio of 1: (1.6-1.8): (0.5-0.6) carrying out acid leaching, and carrying out heat preservation reaction for 8 hours after acid is added, wherein the mass concentration of hydrofluoric acid is 55%, the mass concentration of sulfuric acid is 98%, and acid leaching liquid is obtained;
(2) Adjusting the acidity of the acid leaching solution to HF 6.8-7.0 mol/L by using hydrofluoric acid and sulfuric acid, and adjusting the pH to H2SO43.8-3.9 mol/L, carrying out countercurrent extraction in a 10-grade extraction tank by using octanol as an extractant, wherein the volume ratio of an organic phase to a water phase is 1.2:1, and obtaining a tantalum-niobium-containing organic phase;
(3) preparing a pickling agent with the concentration of 3.7 mol/L by using 98% CP pure sulfuric acid, wherein the volume ratio of the tantalum-niobium-containing organic phase to the pickling agent is 2.5:1, and carrying out 10-stage countercurrent washing to obtain an acid-washed organic phase;
(4) Preparing 4 mol/L and 3mol/L sulfuric acid solutions by using 98% CP pure sulfuric acid as niobium-removing agents of the first-stage niobium-removing agent and the second-stage niobium-removing agent respectively, and extracting tantalum through the first-stage 15-grade niobium-removing agent, the second-stage 10-grade niobium-removing agent and the 10-grade tantalum-removing agent to obtain a first-stage niobium solution and a second-stage niobium solution;
(5) and (3) respectively introducing ammonia gas into the two sections of niobium-containing solutions to neutralize the solutions until the pH value is 9, and washing, drying and calcining the solutions by pure water to obtain a high-purity niobium oxide product and a common niobium oxide product.
Through detection, the main component Nb of the product in the high-purity niobium oxide2O599.994 percent, 3.8ppm of impurity tantalum, 3.1ppm of iron and 6.1ppm of stibium, and other impurities can all meet the non-ferrous metal industry standard FNb2O5The requirement of 04 grades, the specific element components are shown in Table 2, the mass of the high-purity niobium oxide product is 285kg, the mass of the common niobium oxide product is 132kg, and the mass ratio is 2.16: 1.
EXAMPLE III
(1) 1000kg of niobium-tantalum-iron ore crushed to 300 meshes is treated with hydrofluoric acid and sulfuric acid according to a solid-to-liquid ratio of 1: (1.6-1.8): (0.5-0.6) carrying out acid leaching, and carrying out heat preservation reaction for 8 hours after acid is added, wherein the mass concentration of hydrofluoric acid is 55%, the mass concentration of sulfuric acid is 98%, and acid leaching liquid is obtained;
(2) Adjusting the acidity of the acid leaching solution to HF 6.8-7.0 mol/L by using hydrofluoric acid and sulfuric acid, and adjusting the pH to H2SO43.8-3.9 mol/L, carrying out countercurrent extraction in a 20-grade extraction tank by using octanol as an extractant, wherein the volume ratio of an organic phase to a water phase is 1.2:1, and obtaining a tantalum-niobium-containing organic phase;
(3) Preparing a pickling agent with the concentration of 3.8mol/L by using 98% CP pure sulfuric acid, wherein the volume ratio of the tantalum-niobium-containing organic phase to the pickling agent is 2.5:1, and carrying out 10-stage countercurrent washing to obtain an acid-washed organic phase;
(4) Preparing 4.2mol/L and 3mol/L sulfuric acid solutions by using 98% CP pure sulfuric acid as niobium-removing agents of the first-stage niobium-removing agent and the second-stage niobium-removing agent respectively, and extracting tantalum through the first-stage 10-grade niobium-removing agent, the second-stage 10-grade niobium-removing agent and the 10-grade tantalum-removing agent to obtain a first-stage niobium solution and a second-stage niobium solution;
(5) And (3) respectively introducing ammonia gas into the two sections of niobium-containing solutions to neutralize the solutions until the pH value is 9, and washing, drying and calcining the solutions by pure water to obtain a high-purity niobium oxide product and a common niobium oxide product.
through detection, the high-purity niobium oxideThe main component of the medium product is Nb2O599.996 percent, 2.6ppm of impurity tantalum, 2.9ppm of iron and 4.8ppm of stibium, and other impurities can all meet the non-ferrous metal industry standard FNb2O5The requirement of a mark 04 is shown in the table 2, the specific element components are 281kg of the mass of the high-purity niobium oxide product, 137kg of the mass of the common niobium oxide product, and the mass ratio is 2.05: 1.
TABLE 2 EXAMPLES 1-3 high purity niobium oxide chemical compositions (in weight percent)
as can be seen from Table 2, the high purity niobium oxides obtained in examples one to three had lower contents of the respective impurity elements than FNb2O5the standard of-04 shows that the method provided by the invention can fully remove the elements of iron and antimony in the niobium-tantalum-iron ore, the purity of the obtained high-purity niobium oxide is more than or equal to 99.99%, and the market demand for the high-purity niobium oxide is met.
According to the embodiment, the method for preparing the low-antimony low-iron niobium oxide from the niobium-tantalum-iron ore is characterized in that a first-stage niobium-resisting process is added on the basis of the existing process, and a high-niobium solution and a normal-niobium solution are respectively prepared by controlling the acidity of two stages of niobium resisting, wherein the niobium oxide produced by the first-stage niobium solution meets the technical index characteristics of optical wave-grade high-purity niobium oxide, Sb is less than or equal to 10ppm, Fe is less than or equal to 5ppm, the niobium oxide produced by the second-stage niobium solution is common niobium oxide, meets the technical index characteristics of the niobium oxide for ceramics, and the mass ratio of the high-purity niobium oxide to the common niobium oxide is more than or equal to 2. The method provided by the invention can be used for producing the low-antimony low-iron optical wave-level high-purity niobium oxide by utilizing the niobium-tantalum-iron ore, is simple to operate and is easy for industrial production.
Claims (6)
1. A method for preparing low-antimony low-iron high-purity niobium oxide from niobium tantalite is characterized by comprising the following steps of:
(1) Grinding niobium-tantalum-iron ore by an ore grinder, and then decomposing by acid;
(2) After adjusting the acid, the decomposition liquid is extracted by an organic solvent, and metal ions such as tantalum, niobium, antimony, iron and the like enter an organic phase;
(3) removing impurities of an organic phase of fluoroniobate or fluorotantalic acid containing metal ions such as antimony, iron and the like by using a pickling agent to obtain a tantalum-containing niobate washing organic phase;
(4) performing two-stage niobium removal on the tantalum-containing niobate washing organic matter obtained in the step (3) by using a niobium removal agent to obtain two-stage niobium solution;
(5) and (4) respectively introducing ammonia into the two sections of niobium liquid obtained in the step (4) for mixing, carrying out neutralization reaction to generate niobium hydroxide precipitate, and sequentially filtering, washing, drying and calcining to obtain the low-antimony low-iron niobium oxide and the high-antimony high-iron niobium oxide.
2. The method for preparing the niobium oxide with low antimony and low iron and high purity from niobium tantalite according to claim 1, wherein the acid used for acid decomposition in the step (1) is one or two of hydrofluoric acid and sulfuric acid.
3. The method for preparing the niobium oxide with low antimony, low iron and high purity from niobium tantalite according to claim 1, wherein the organic solvent for extraction in step (2) is sec-octanol or methyl isobutyl ketone.
4. The method for preparing the niobium oxide with low antimony and low iron and high purity from niobium tantalite as claimed in claim 1, wherein the acid-washing agent for acid-washing in the step (3) is a sulfuric acid solution with a concentration of 3.5-3.9 mol/L.
5. the method for preparing the niobium oxide with low antimony and low iron and high purity from niobium tantalite according to claim 1, wherein the anti-niobium agent in the step (4) is inorganic acid, which is one or two of hydrofluoric acid and sulfuric acid, preferably sulfuric acid; the two-stage niobium is H-containing in the first stage+One or two of hydrofluoric acid and sulfuric acid of 3-5mol/L are used as anti-niobium agent, and H is preferably contained+4.2mol/L dilute sulfuric acid, and the second stage adopts H-containing+2.8-3.3mol/L of hydrofluoric acid or sulfuric acid or both are used as anti-niobium agent, and H is preferably contained+3mol/L dilute sulfuric acid.
6. The method for preparing the niobium oxide with low antimony and iron content and high purity from the niobium tantalite as claimed in claim 1, wherein the ammonia is introduced in the step (5) in the form of one of ammonia water, ammonia gas and liquid ammonia; the purity of the high-purity niobium oxide is more than or equal to 99.99 percent.
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Application publication date: 20191213 |