Method for high-efficiency purification and directional oxygen removal and impurity removal of antimony-rich alloy

Abstract

The application belongs to the technical field of metallurgy, and relates to a method for efficiently purifying and directionally removing oxygen and impurities from a precious antimony alloy, which comprises the following steps: S1, after the precious antimony alloy is melted, an arsenic-tellurium removal agent is added, and smelting is performed at 600-610 DEG C to obtain a pre-impurity removal alloy melt and an arsenic-tellurium residue; the arsenic-tellurium removal agent is a mixture of sodium hydroxide and sodium nitrate; S2, the pre-impurity removal alloy melt obtained in step S1 is heated to 620-640 DEG C, a reducing agent is added, and smelting is performed to obtain an arsenic alkali residue and a refined antimony alloy; the reducing agent is a mixture of antimony sulfide and sodium hydroxide; S3, the arsenic-tellurium residue obtained in step S1 and the arsenic alkali residue obtained in step S2 are ball milled, leaching and filtration are performed to obtain a filtrate and a filter residue; S4, the filtrate obtained in step S3 is mixed with sulfuric acid, and after reaction, a neutralization residue and a neutralization liquid are obtained. By introducing the efficient arsenic-tellurium removal agent and the reducing agent, the content of antimony in the arsenic alkali residue is significantly reduced, and the direct recovery rate of antimony and the recovery rate of tellurium are effectively improved.

Description

Technical Field

[0001] This invention belongs to the field of metallurgical technology, specifically relating to a method for efficient purification and targeted oxygen suppression and impurity removal of precious antimony alloys. Background Technology

[0002] Antimony is an important metalloid element with unique physical and chemical properties, widely used in flame retardants, alloy manufacturing, semiconductors, and pharmaceuticals, playing an indispensable role in modern industry. In flame retardant applications, antimony is primarily used to produce antimony white (antimony trioxide). Currently, the raw materials for antimony white production mainly include lead anode mud, antimony ingots, and other antimony-containing materials. The preparation process generally involves: first, obtaining precious antimony through reduction smelting of antimony-containing materials; then, removing impurities such as arsenic and tellurium through a purification process; and finally, obtaining qualified antimony white products through blowing.

[0003] In the process of removing impurities from precious antimony, traditional methods typically employ alkali addition to remove arsenic and tellurium. However, this process has significant shortcomings: the resulting arsenic-alkali slag has a high antimony content, resulting in low antimony recovery. Simultaneously, tellurium is dispersed and of low grade, failing to achieve effective enrichment. To improve antimony recovery, the material is often repeatedly smelted, leading to the continuous accumulation of arsenic within the system. The lack of effective open-circuit treatment negatively impacts the overall economic efficiency and environmental friendliness of the process. Summary of the Invention

[0004] To address the shortcomings of existing technologies, this invention provides a method for the efficient purification and targeted oxygen suppression and impurity removal of precious antimony alloys. By introducing a highly efficient arsenic and tellurium removal agent and a composite reducing agent, efficient separation and separate recovery of arsenic, tellurium, and antimony are achieved. This method significantly reduces the antimony content in arsenic-alkali slag while simultaneously enriching tellurium, effectively improving the direct antimony recovery rate and tellurium recovery rate during the preparation of antimony white from precious antimony alloys. It has promising prospects for industrial application and significant promotional value.

[0005] The specific technical solution is as follows:

[0006] A method for efficient purification and targeted oxygen suppression and impurity removal of noble antimony alloys includes the following steps:

[0007] S1 After melting the noble antimony alloy, an arsenic and tellurium removal agent is added, and the alloy is smelted at 600~610℃ to obtain a pre-purified alloy melt and arsenic and tellurium slag; the arsenic and tellurium removal agent is a mixture of sodium hydroxide and sodium nitrate.

[0008] S2 The pre-purified alloy melt obtained in step S1 is heated to 620~640℃, a reducing agent is added, and arsenic-alkali slag and refined antimony alloy are obtained by smelting; the reducing agent is a mixture of antimony sulfide and sodium hydroxide.

[0009] S3 The arsenic tellurium slag obtained in step S1 and the arsenic alkali slag obtained in step S2 are ball-milled, leached and filtered to obtain filtrate and filter residue;

[0010] S4. The filtrate obtained in step S3 is mixed with sulfuric acid, and after the reaction, neutralization residue and neutralization liquid are obtained.

[0011] Among them, the noble antimony alloy is an alloy obtained from the reduction smelting of lead anode mud in a converter. Its main components are: Cu content 0.3wt%~0.7wt%, Sb content 55wt%~65wt%, Au content 900~1300g / t, Ag content 5wt%~15wt%, Pb content 8wt%~20wt%, Bi content 5wt%~20wt%, As content 3wt%~10wt%, and Te content 0.5wt%~5wt%.

[0012] The reaction mechanism of this invention is as follows:

[0013] This invention first removes most of the arsenic and tellurium from the noble antimony alloy at a relatively low temperature (600~610℃) using an arsenic and tellurium removal agent, causing the arsenic and tellurium slag to float on the surface of the pre-removed noble antimony alloy melt. Then, at a higher temperature (620~640℃), a reducing agent is used for deep arsenic removal, and crucially, the oxidation of metallic antimony is directionally inhibited. This invention achieves deep reduction of antimony and recovery of arsenic and tellurium, avoiding antimony dispersion during the impurity removal process and thus improving the direct antimony recovery rate.

[0014] In step S1, sodium nitrate acts as an oxidant to oxidize arsenic and tellurium in the noble antimony alloy into arsenates and tellurates, which then react with sodium hydroxide to form arsenic-tellurium slag, thereby achieving efficient enrichment of tellurium. The main reaction is as follows:

[0015] 2NaNO3→2NaNO2+O2↑;

[0016] As2O3 + O2 → As2O5;

[0017] As2O5+6NaOH→2Na3AsO4+3H2O;

[0018] Te + O2 → TeO2;

[0019] 2TeO2 + 1 / 2O2 → Te2O5;

[0020] Te2O5+6NaOH→2Na3TeO4+3H2O;

[0021] 3As2O3+3Te+15NaNO3+24NaOH→6Na3AsO4+3Na2TeO4+15NaNO2+12H2O.

[0022] Preferably, in step S1, the melting temperature is 600~610℃.

[0023] Preferably, in step S1, the melting time is 4-5 hours, until the surface alloy turns slightly red, at which point the melting is stopped.

[0024] Preferably, in step S1, the molar ratio of the arsenic removal agent, sodium hydroxide, and sodium nitrate is (250~260):(7~10).

[0025] Preferably, in step S1, the molar ratio of sodium hydroxide in the arsenic and tellurium removal agent to the total amount of arsenic and tellurium in the noble antimony alloy is 1:(1.5~3).

[0026] In step S2, a mixture of antimony sulfide and sodium hydroxide is used as a reducing agent. Antimony sulfide preferentially combines with oxygen, forming a protective layer on the surface of the molten antimony through a chemical reaction. This directionally inhibits the oxidation of the main antimony metal, keeping it within the alloy and preventing it from entering the slag phase. Meanwhile, the impurity arsenic is deeply reduced and removed. The main reactions are as follows:

[0027] 2Sb2S3+9O2→2Sb2O3+6SO2↑;

[0028] Sb₂O₃ + 2NaOH → 2NaSbO₂ + H₂O;

[0029] As2O3+Sb2S3→As2S3+Sb2O3.

[0030] Preferably, in step S2, the melting time is 4-5 hours, until the alloy turns silvery-white.

[0031] Preferably, in step S2, the molar ratio of the reducing agent, antimony sulfide, and sodium hydroxide is (1~4):(82~88).

[0032] Preferably, in step S2, the molar ratio of sodium hydroxide in the reducing agent to the total amount of arsenic in the pre-purified alloy melt is 1:(1~3).

[0033] Preferably, in step S2, the refined antimony alloy is blown to obtain antimony white.

[0034] In step S3, the arsenic-tellurium slag and arsenic-alkali slag are ball-milled to leach arsenic and tellurium from the slag.

[0035] Preferably, in step S3, the ball milling is performed to a particle size of 100-200 mesh; during the leaching process, the liquid-solid mass ratio is (3-4):1, the leaching temperature is 70-80℃, and the leaching time is 30-60 min.

[0036] Preferably, the filter residue obtained in step S3 is returned to the converter for processing to recover valuable metals.

[0037] In step S4, sulfuric acid is used for a neutralization reaction to convert the tellurium-containing compounds in the filtrate into crude tellurium dioxide, i.e., neutralization residue, which is then separated from the arsenic in the neutralization liquid.

[0038] Preferably, in step S4, the sulfuric acid concentration is 8wt%~12wt%.

[0039] Preferably, in step S4, the molar ratio of sulfuric acid to the total amount of tellurium in the filtrate is 1:(1~3), and the reaction time is 0.5~1h.

[0040] Preferably, the neutralized liquid obtained in step S4 is returned to the water treatment system to recover arsenic, and the neutralized residue is used to recover tellurium.

[0041] Compared with the prior art, the present invention has the following beneficial effects:

[0042] This invention introduces a highly efficient arsenic and tellurium removal agent and a composite reducing agent during the impurity removal process of precious antimony alloys. On the one hand, it achieves the enrichment and recovery of tellurium, avoiding the problem of low yield caused by the dispersion of tellurium during recovery. On the other hand, it prevents antimony-containing compounds from entering the arsenic-alkali slag, thereby improving the direct recovery rate of antimony. At the same time, this invention has strong applicability to the impurity removal of precious antimony alloys and reduces the number of repeated treatments during the impurity removal process, thus lowering production costs. Attached Figure Description

[0043] Figure 1 This is a process flow diagram of the method for efficient purification and targeted oxygen suppression and impurity removal of noble antimony alloys in a specific implementation. Detailed Implementation

[0044] The embodiments of the present invention will be described in further detail below with reference to the accompanying drawings and examples. The following examples are for illustrative purposes only and should not be construed as limiting the scope of the invention. Unless otherwise specified, the experimental methods used in the following examples are conventional methods. Unless otherwise specified, the materials and reagents used in the following examples are commercially available.

[0045] Example 1

[0046] A method for efficient purification and targeted oxygen suppression and impurity removal of precious antimony alloys.

[0047] The noble antimony alloy is derived from the alloy obtained by reduction smelting of lead anode mud in a converter. Its main components are: Cu content 0.65wt%, Sb content 60.66wt%, Au content 1201g / t, Ag content 9.86wt%, Pb content 13.67wt%, Bi content 6.46wt%, As content 6.55wt%, and Te content 1.55wt%.

[0048] Includes the following steps:

[0049] S1 20,000 kg of noble antimony alloy was put into a refining pot and melted at 600°C. Unmelted slag was removed, stirring was started, and a mixture of sodium hydroxide and sodium nitrate was added. The mixture was stirred continuously and smelted at 600°C for 4.5 hours to obtain pre-removed impurity alloy melt and 2297 kg of arsenic and tellurium slag. The molar ratio of sodium hydroxide to sodium nitrate was 255:8, and the molar ratio of sodium hydroxide to the total amount of arsenic and tellurium in the arsenic and tellurium removal agent was 1:1.5.

[0050] S2 The pre-purified alloy melt obtained in step S1 is heated to 630°C, and a mixture of antimony sulfide and sodium hydroxide is added. After continuous stirring, it is smelted for 4.5 hours to obtain 2170 kg of arsenic-alkali slag and refined antimony alloy. The refined antimony alloy is then transferred to an oxidation pot and blown to produce qualified antimony white. The molar ratio of antimony sulfide to sodium hydroxide is 2:85, and the molar ratio of sodium hydroxide to the total amount of arsenic in the pre-purified alloy melt is 1:2.

[0051] S3 The arsenic tellurium slag obtained in step S1 and the arsenic alkali slag obtained in step S2 are ball-milled to a particle size of 200 mesh, and then leached with deionized water for 60 min at 80°C and a liquid-solid mass ratio of 3:1. After filtration, filtrate and filter residue are obtained, and the filter residue is returned to the converter for processing to recover valuable metals.

[0052] S4 The filtrate obtained in step S3 is mixed with dilute sulfuric acid with a concentration of 10wt%, and reacted for 1 hour to obtain 600 kg of crude tellurium dioxide neutralization residue and neutralization liquid. The neutralization liquid is returned to the water treatment system to recover arsenic, and the neutralization residue is recovered to obtain tellurium ingots. The molar ratio of sulfuric acid to the total amount of tellurium in the filtrate is 1:1.

[0053] Example 2

[0054] A method for efficient purification and targeted oxygen suppression and impurity removal of precious antimony alloys.

[0055] The noble antimony alloy is derived from the alloy obtained by reduction smelting of lead anode mud in a converter. Its main components are: Cu content 0.48wt%, Sb content 60.01wt%, Au content 1155g / t, Ag content 9.63wt%, Pb content 13.12wt%, Bi content 6.32wt%, As content 6.15wt%, and Te content 1.61wt%.

[0056] Includes the following steps:

[0057] S1 20,000 kg of noble antimony alloy was put into a refining pot and melted at 605°C. Unmelted slag was removed, stirring was started, and a mixture of sodium hydroxide and sodium nitrate was added. The mixture was stirred continuously and smelted at 605°C for 4 hours to obtain pre-removed impurity alloy melt and 2,072 kg of arsenic and tellurium slag. The molar ratio of sodium hydroxide to sodium nitrate was 250:7, and the molar ratio of sodium hydroxide to the total amount of arsenic and tellurium in the arsenic and tellurium removal agent was 1:2.

[0058] S2 The pre-purified alloy melt obtained in step S1 is heated to 620°C, and a mixture of antimony sulfide and sodium hydroxide is added. After continuous stirring, it is smelted for 4 hours to obtain 2212 kg of arsenic-alkali slag and refined antimony alloy. The refined antimony alloy is then transferred to an oxidation pot and blown to produce qualified antimony white. The molar ratio of antimony sulfide to sodium hydroxide is 1:82, and the molar ratio of sodium hydroxide to the total amount of arsenic in the pre-purified alloy melt is 1:1.

[0059] S3 The arsenic tellurium slag obtained in step S1 and the arsenic alkali slag obtained in step S2 are ball-milled to a particle size of 150 mesh, and then leached with deionized water for 50 min at 75°C and a liquid-solid mass ratio of 3.5:1. After filtration, filtrate and filter residue are obtained, and the filter residue is returned to the converter for processing to recover valuable metals.

[0060] S4 The filtrate obtained in step S3 is mixed with dilute sulfuric acid with a concentration of 12wt%, and reacted for 0.5h to obtain 584kg of crude tellurium dioxide neutralization residue and neutralization liquid. The neutralization liquid is returned to the water treatment system to recover arsenic, and the neutralization residue is recovered to obtain tellurium ingots. The molar ratio of sulfuric acid to the total amount of tellurium in the filtrate is 1:3.

[0061] Example 3

[0062] A method for efficient purification and targeted oxygen suppression and impurity removal of precious antimony alloys.

[0063] The noble antimony alloy is derived from the alloy obtained by reduction smelting of lead anode mud in a converter. Its main components are: Cu content 0.45wt%, Sb content 59.65wt%, Au content 1265g / t, Ag content 9.45wt%, Pb content 15.12wt%, Bi content 6.98wt%, As content 5.82wt%, and Te content 1.49wt%.

[0064] Includes the following steps:

[0065] S1 20000 kg of noble antimony alloy is put into a refining pot and melted at 610℃. Unmelted slag is removed, stirring is started, and a mixture of sodium hydroxide and sodium nitrate is added. The mixture is stirred continuously and smelted at 610℃ for 5 hours to obtain pre-removed impurity alloy melt and 2035 kg of arsenic and tellurium slag. The molar ratio of sodium hydroxide to sodium nitrate is 260:10, and the molar ratio of sodium hydroxide to the total amount of arsenic and tellurium in the arsenic and tellurium removal agent is 1:3.

[0066] S2 The pre-purified alloy melt obtained in step S1 is heated to 640°C, and a mixture of antimony sulfide and sodium hydroxide is added. After continuous stirring, it is smelted for 5 hours to obtain 2103 kg of arsenic-alkali slag and refined antimony alloy. The refined antimony alloy is then transferred to an oxidation pot and blown to produce qualified antimony white. The molar ratio of antimony sulfide to sodium hydroxide is 4:88, and the molar ratio of sodium hydroxide to the total amount of arsenic in the pre-purified alloy melt is 1:3.

[0067] S3 The arsenic tellurium slag obtained in step S1 and the arsenic alkali slag obtained in step S2 are ball-milled to a particle size of 100 mesh, and then leached with deionized water for 30 minutes at 70°C and a liquid-solid mass ratio of 4:1. After filtration, filtrate and filter residue are obtained, and the filter residue is returned to the converter for processing to recover valuable metals.

[0068] S4 The filtrate obtained in step S3 is mixed with dilute sulfuric acid with a concentration of 8wt%, and reacted for 0.8h to obtain 593kg of crude tellurium dioxide neutralization residue and neutralization liquid. The neutralization liquid is returned to the water treatment system to recover arsenic, and the neutralization residue is recovered to obtain tellurium ingots. The molar ratio of sulfuric acid to the total amount of tellurium in the filtrate is 1:2.

[0069] Comparative Example 1

[0070] A method for efficient purification and targeted oxygen suppression and impurity removal of precious antimony alloys.

[0071] The noble antimony alloy is derived from the alloy obtained by reduction smelting of lead anode mud in a converter. Its main components are: Cu content 0.65wt%, Sb content 59.12wt%, Au content 1181g / t, Ag content 9.82wt%, Pb content 13.32wt%, Bi content 6.56wt%, As content 6.62wt%, and Te content 1.52wt%.

[0072] Includes the following steps:

[0073] S1 20000 kg of noble antimony alloy is put into a refining pot and melted at 610°C. Unmelted slag is removed, stirring is started, sodium hydroxide is added, stirring is continued, and smelting is carried out at 610°C for 5 hours to obtain pre-removed impurity alloy melt and 2685 kg of arsenic and tellurium slag; wherein, the molar ratio of sodium hydroxide in the arsenic and tellurium removal agent to the total amount of arsenic and tellurium in the noble antimony alloy is 1:3;

[0074] S2 The pre-purified alloy melt obtained in step S1 is heated to 640°C, sodium hydroxide is added, and the mixture is stirred continuously. After smelting for 5 hours, 2702 kg of arsenic-alkali slag and refined antimony alloy are obtained. The refined antimony alloy is then transferred to an oxidation pot and blown to produce qualified antimony white. The molar ratio of sodium hydroxide in the reducing agent to the total amount of arsenic in the pre-purified alloy melt is 1:3.

[0075] S3 The arsenic tellurium slag obtained in step S1 and the arsenic alkali slag obtained in step S2 are ball-milled to a particle size of 100 mesh, and then leached with deionized water for 30 minutes at 70°C and a liquid-solid mass ratio of 4:1. After filtration, filtrate and filter residue are obtained, and the filter residue is returned to the converter for processing to recover valuable metals.

[0076] S4 The filtrate obtained in step S3 is mixed with dilute sulfuric acid with a concentration of 8wt%, and reacted for 0.8h to obtain 200kg of crude tellurium dioxide neutralization residue and neutralization liquid. The neutralization liquid is returned to the water treatment system to recover arsenic, and the neutralization residue is recovered to obtain tellurium ingots. The molar ratio of sulfuric acid to the total amount of tellurium in the filtrate is 1:2.

[0077] Comparative Example 2

[0078] Referring to Example 1, the difference is that sodium nitrate is not added in step S1; wherein, the amount of arsenic tellurium slag is 2567 kg, the amount of arsenic alkali slag is 2281 kg, and the amount of crude tellurium dioxide neutralization slag is 325 kg.

[0079] Comparative Example 3

[0080] Referring to Example 1, the difference is that antimony sulfide is not added in step S2; wherein, the amount of arsenic tellurium slag is 2103 kg, the amount of arsenic alkali slag is 2682 kg, and the amount of crude tellurium dioxide neutralization slag is 298 kg.

[0081] test

[0082] The component content of the arsenic tellurium slag, arsenic alkali slag and crude tellurium dioxide neutralization slag obtained in Examples 1-3 and Comparative Examples 1-3 was detected, and the results are shown in Table 1.

[0083] The composition of arsenic tellurium slag, arsenic alkali slag, and crude tellurium dioxide neutralization slag was determined by inductively coupled plasma atomic emission spectrometry (YS / T 227.12-2011).

[0084] Table 1. Composition content of arsenic tellurium slag, arsenic-alkali slag, and neutralization slag

[0085]

[0086] Note: "-" in Table 1 indicates not detected.

[0087] Characterization results from Example 1 show that by adding the arsenic-removing tellurium agent, tellurium is effectively enriched, and the tellurium recovery rate (i.e., the percentage of tellurium content in the neutralized slag to the total tellurium content in the noble antimony alloy) reaches 67.85%. Furthermore, the reducing agent of this invention can deeply remove arsenic from the noble antimony alloy and inhibit antimony removal, reducing the antimony content in the arsenic-alkali slag to 0.99% of the total antimony content in the noble antimony alloy, thus improving the direct antimony recovery rate. Correspondingly, in Example 2, the tellurium recovery rate is 67.56%, and the antimony content in the arsenic-alkali slag accounts for 0.89% of the total antimony content in the noble antimony alloy; in Example 3, the tellurium recovery rate is 72.65%, and the antimony content in the arsenic-alkali slag accounts for 0.90% of the total antimony content in the noble antimony alloy. In contrast, in Comparative Example 1, because only sodium hydroxide was added in steps S1 and S2, the tellurium recovery rate was only 11.2%, and the antimony content in the arsenic-alkali slag accounted for 6.01% of the antimony content in the precious antimony alloy, increasing the amount of antimony occupied in the arsenic-alkali slag and reducing the direct antimony recovery rate. In Comparative Example 2, because only sodium hydroxide was added in step S1, the tellurium recovery rate was only 21.1%, and the antimony content in the arsenic-alkali slag accounted for 3.74% of the antimony content in the precious antimony alloy; in Comparative Example 3, because only sodium hydroxide was added in step S2, the tellurium recovery rate was only 20.6%, and the antimony content in the arsenic-alkali slag accounted for 5.33% of the antimony content in the precious antimony alloy. Therefore, this invention, by adding an arsenic and tellurium removal agent, converts tellurium and arsenic in the precious antimony alloy into oxidized salt slag, significantly improving the enrichment and recovery of tellurium. At the same time, the reducing agent of this invention deeply removes arsenic from the precious antimony alloy and inhibits the removal of antimony, reducing the antimony content in the arsenic-alkali slag and improving the direct antimony recovery rate.

[0088] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for high-efficiency purification and directional oxygen removal and impurity removal of a precious antimony alloy, characterized in that, It comprises the following steps: S1, after melting the noble antimony alloy, adding arsenic tellurium removal agent, melting at 600-610℃ to obtain a pre-removal alloy melt and arsenic tellurium slag; the arsenic tellurium removal agent is a mixture of sodium hydroxide and sodium nitrate; S2, the pre-removal alloy melt obtained in step S1 is heated to 620-640℃, and a reducing agent is added, and the arsenic alkali slag and refined antimony alloy are obtained by smelting; the reducing agent is a mixture of antimony sulfide and sodium hydroxide; S3, the arsenic tellurium slag obtained in step S1 and the arsenic alkali slag obtained in step S2 are ball milled, leached and filtered to obtain a filtrate and a filter residue; S4, the filtrate obtained in step S3 is mixed with sulfuric acid, and the neutralization slag and the neutralization liquid are obtained after reaction; In step S1, the molar ratio of sodium hydroxide to sodium nitrate in the arsenic tellurium removal agent is (250-260):(7-10); in step S1, the molar ratio of sodium hydroxide in the arsenic tellurium removal agent to the total amount of arsenic and tellurium in the noble antimony alloy is 1:(1.5-3); in step S2, the molar ratio of sodium hydroxide to the total amount of arsenic in the reducing agent is (1-4):(82-88).

2. The method of claim 1, wherein, In step S1, the smelting time is 4-5h.

3. The method of claim 1, wherein, In step S2, the smelting time is 4-5h.

4. The method of claim 1, wherein, In step S2, the molar ratio of sodium hydroxide in the reducing agent to the total amount of arsenic in the pre-removal alloy melt is 1:(1-3).

5. The method of claim 1, wherein, In step S3, the particle size is 100-200 mesh after ball milling; in the leaching process, the liquid-solid mass ratio is (3-4):1, the leaching temperature is 70-80℃, and the leaching time is 30-60min.

6. The method of claim 1, wherein, In step S4, the concentration of sulfuric acid is 8wt%-12wt%.

7. The method of claim 1, wherein, In step S4, the molar ratio of sulfuric acid to the total amount of tellurium in the filtrate is 1:(1-3), and the reaction time is 0.5-1h.

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