CN114920208B - Method for efficiently separating tellurium or separating tellurium and selenium from tellurium-containing material - Google Patents
Method for efficiently separating tellurium or separating tellurium and selenium from tellurium-containing material Download PDFInfo
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Abstract
A method for efficiently separating tellurium from tellurium-containing materials comprises the following steps: adding tellurium-containing materials into an alkaline vulcanization system solution for leaching, and carrying out solid-liquid separation to obtain tellurium-containing leaching solution and leaching residues; wherein, the alkaline vulcanization system solution is mainly a mixed solution prepared from sodium sulfide, sodium hydroxide and sublimed sulfur; adding sodium sulfite into the leaching solution to react to obtain tellurium precipitation slag and tellurium precipitation post-liquid; washing and filtering the tellurium precipitation slag to obtain coarse tellurium powder. Further, the invention also discloses a method for preparing the selenium-precipitating solution by adding an oxidant into the tellurium-precipitating solution for reaction, adjusting the pH value of the solution to 1-2 after the reaction is finished, adding sodium sulfite for reaction, and filtering to obtain selenium-precipitating slag and selenium-precipitating solution; washing and filtering the selenium-precipitating slag to obtain crude selenium powder. The method adopts an alkaline vulcanization system solution composed of sodium sulfide, sodium hydroxide and sublimed sulfur to leach tellurium-containing materials, can realize the efficient separation and extraction of valuable metals such as tellurium, selenium and the like, and enriches heavy metal ions such as copper, lead, bismuth and the like in leaching slag, so that the selective extraction effect is good.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a method for efficiently separating tellurium or separating tellurium and selenium from tellurium-containing materials.
Background
Tellurium is a typical scattered metal, is known as a vitamin for modern industry, national defense and advanced technology, is a supporting raw material of modern high and new technology materials, and is an essential key metal for development of strategic emerging industry in China. Tellurium and its compounds have excellent photoelectric characteristics, and are widely used in solar cells, thermoelectric materials and semiconductor devices, and demand for them is increasing.
Tellurium-containing materials produced in the copper/lead anode slime oxidation refining process are main materials for extracting tellurium, and the ratio of the tellurium-containing materials is more than 90%. Because of different anode slime treatment processes of various enterprises, tellurium-containing materials are various, have complex phases and valuable goldThe method belongs to copper telluride slag, tellurium slag and flotation tailings, and has large content fluctuation. Copper telluride slag mainly comes from a copper-tellurium removal process in the copper anode slime treatment process, and at present copper anode slime treatment enterprises can produce the slag, so that the copper telluride slag becomes the most main tellurium extraction raw material. Tellurium slag mainly originates from a pyrogenic process treatment process of copper and lead anode slime and a crude bismuth alkaline refining process, and the method for recovering tellurium from the tellurium slag mainly comprises an alkaline leaching method, a pressurized alkaline leaching method, an acid leaching method, a pressurized acid leaching method, copper powder replacement method, a chlorination method, a solvent extraction method and the like. The flotation tailings are mainly derived from the copper anode slime treatment process by adopting a dressing and smelting combined process developed by the Yunnan copper industry limited company, and the research of extracting tellurium by taking the slag as a raw material is relatively less in China at present. The alkaline leaching method is a main method for recycling tellurium by various copper and lead smelting enterprises nationwide at present, sodium hydroxide is utilized to leach sodium tellurite, tellurium dioxide and the like in tellurium slag into solution, and tellurium ingot products (99.99%) are obtained through purification, impurity removal, neutralization and tellurium precipitation, alkali dissolution and liquid making and electrolysis. The method is mature and stable, and has good product quality, but has low adaptability to Na 2 TeO 3 The main tellurium-containing materials have better adaptability, but have poorer tellurium-containing material treatment effects on telluride, simple substance tellurium and indissolvable tellurate), long process flow, low tellurium recovery rate (60-70 percent) and the like.
The alkaline sulfuration leaching is an important hydrometallurgical separation method, is widely applied to high-efficiency separation of metals such as tellurium, arsenic, tin and the like, and has the technical advantages of strong selectivity and high separation efficiency. At present, the method has relatively few researches on separating and recovering tellurium from tellurium-containing solid wastes. In the patent document with publication No. CN104762471A, there is disclosed a method for strengthening leaching of tellurium slag, two or three of sodium sulfide, sodium sulfite and sodium thiosulfate are prepared into solution, tellurium slag is added into the solution according to a certain liquid-solid ratio, nitrogen is introduced as protective atmosphere, and MeTeO is carried out under high temperature and high pressure 3 And MeTeO 4 Conversion of the insoluble substances to soluble Na 2 TeO 3 And making heavy metal ions of the solution generate MeS precipitate, allowing the MeS precipitate to enter leaching residues, and finally, performing vacuum filtration to realize solid-liquid separation. The method needs to leach tellurium under high temperature and high pressure, and has high energy consumption, complex and dangerous operation and raw materialsThe production cost is high. Patent document CN106636661a discloses a method for selectively separating and recovering tellurium from tellurium slag, wherein tellurium slag is added into sodium sulfide solution, stirred and leached, and sodium sulfite is added into the obtained leaching solution to reduce to obtain crude tellurium. The method has good separation effect, high selectivity and simple process, but has poor raw material adaptability, and is not suitable for treating tellurium-containing materials such as copper telluride slag, flotation tailings and the like.
In summary, the different anode slime treatment processes result in various tellurium-containing materials, and the current treatment process cannot realize the centralized treatment of different types of tellurium-containing materials, so that the tellurium production scale is smaller, and stable supply to the upstream market cannot be satisfied. Therefore, development of a method for efficiently separating tellurium from tellurium-containing materials of different types, which has strong raw material adaptability and is easy to popularize and apply on a large scale, is needed.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and providing a method for efficiently separating tellurium from tellurium-containing materials or a method for separating tellurium and selenium, which has strong raw material adaptability and is easy to popularize and apply in a large scale.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for efficiently separating tellurium from tellurium-containing materials, comprising the following steps:
(1) Adding tellurium-containing materials into an alkaline vulcanization system solution for leaching, and carrying out solid-liquid separation to obtain tellurium-containing leaching solution and leaching residues; wherein the alkaline vulcanization system solution is mainly a mixed solution composed of sodium sulfide, sodium hydroxide and sublimed sulfur;
(2) Adding sodium sulfite into the leaching solution to react, and filtering after the reaction is finished to obtain tellurium precipitation slag and tellurium precipitation post-liquid; washing and filtering the tellurium precipitation slag to obtain coarse tellurium powder.
As a general inventive concept, the present invention also provides a method of efficiently separating tellurium and selenium from a tellurium-containing material, comprising the steps of:
(1) Adding tellurium-containing materials into an alkaline vulcanization system solution for leaching, and carrying out solid-liquid separation to obtain tellurium-containing leaching solution and leaching residues; wherein the alkaline vulcanization system solution is mainly a mixed solution composed of sodium sulfide, sodium hydroxide and sublimed sulfur.
(2) Adding sodium sulfite into the leaching solution to react, and filtering after the reaction is finished to obtain tellurium precipitation slag and tellurium precipitation post-liquid; washing and filtering the tellurium precipitation slag to obtain crude tellurium powder;
(3) Adding an oxidant into the tellurium precipitation solution for oxidation reaction, adjusting the pH value of the solution to 1-2 after the reaction is finished, adding sodium sulfite for reaction, and filtering after the reaction is finished to obtain selenium precipitation slag and selenium precipitation solution;
(4) Washing and filtering the selenium-precipitating slag to obtain crude selenium powder.
In the above method, preferably, in the step (1), the leaching temperature is 70-90 ℃, and the solid ratio of the leaching solution is 5-10: 1, the ratio unit is mL/g, and the leaching time is 2-5 h.
In the above method, preferably, in the step (1), the solution excess coefficient of the alkaline vulcanization system is 5 to 10 times. The excess alkaline vulcanizing system solution is in the range, the selenium and tellurium leaching effect is optimal, and the leaching rate of heavy metal ions such as copper is low.
In the above method, preferably, in the step (1), the alkaline vulcanization system solution is prepared by mixing the following components in mass ratio of 1 to 3: 1-2: 1 to 3: 30-50 of sodium sulfide, sublimed sulfur, sodium hydroxide and water, and reacting for 1-3 h at 60-80 ℃.
The ion composition in the alkaline vulcanization system is complex (S 2- 、S a 2- 、S 2 O 3 2- ) When the tellurium-containing material is added into the alkaline vulcanization system, sodium tellurite, tellurium oxide and tellurium oxide will react with S 2- 、S a 2- 、S 2 O 3 2- The plasma reacts to transform it into Te (VI) S x O y 2- And Te (IV) S x O y 2- And leaching, while heavy metal ions such as Cu and the like are precipitated in a MeS form and stored in leaching residues, so that the tellurium is selectively extracted. The main chemical reactions involved are:
Me 2 Te+Na 2 S+3S＝Na 2 TeS 3 +Me 2 S (1)
MeTe+Na 2 S+3S＝Na 2 TeS 3 +MeS (2)
Me 2 Te 3 +3Na 2 S+6S＝3Na 2 TeS 3 +Me 2 S 3 (3)
Te+Na 2 S+2S＝Na 2 TeS 3 (4)
Te+Na 2 S+3S＝Na 2 TeS 4 (5)
TeO 2 +3Na 2 S+2H 2 O＝Na 2 TeS 3 +4NaOH (6)
TeO 2 +3Na 2 S+S+2H 2 O＝Na 2 TeS 3 +4NaOH (7)
Na 2 TeO 3 +3Na 2 S+3H 2 O＝Na 2 TeS 3 +6NaOH (8)
Na 2 TeO 3 +3Na 2 S+S+3H 2 O＝Na 2 TeS 4 +6NaOH (9)
Na 2 TeO 4 +4Na 2 S+4H 2 O＝Na 2 TeS 4 +8NaOH (10)
in the above method, preferably, in the step (2), the sodium sulfite excess coefficient is 5-10 times, the reaction temperature is 30-50 ℃, and the reaction time is 2-5 hours.
In the above method, preferably, in step (2) and step (4), the washing is ultrasonic washing, the washing temperature is 30-50 ℃, and the washing time is 10-30 min. The tellurium slag and selenium slag obtained by directional reduction in the alkaline vulcanization system contain a large amount of sulfur and sodium, so that the product quality is affected, sulfur and sodium impurities in the product can be completely removed after ultrasonic washing, and coarse tellurium powder and coarse selenium powder with higher purity are obtained.
In the above method, preferably, the tellurium-containing material is one or more of copper telluride slag, tellurium slag and flotation tailings. The main phase in the copper telluride slag is CuO, cu 2 O、Cu 5 Te 3 、Cu 2 Te, the main chemical composition is Te, cu, S, cl; the main phase in the flotation tailings is PbSO 4 、BaSO 4 、TeO 2 、PbSbO 6 The main chemical composition is Te, pb, sb, ba, bi, S, C; te in main phase of tellurium slag 2 O 5 、Na 2 SeO 4 、Na 4 PbO 4 The main chemical composition is Te, se, cu, ag, pb, na.
In the above method, preferably, in the step (3), the oxidant is hydrogen peroxide, the hydrogen peroxide excess coefficient is 1-3 times, the reaction temperature is 25-35 ℃, and the reaction time is 1-3 hours.
In the above method, preferably, the sodium sulfite excess coefficient is 3-10 times, the reduction temperature is 30-50 ℃, and the reduction time is 2-5 hours.
Compared with the prior art, the invention has the advantages that:
(1) The method adopts an alkaline vulcanization system solution composed of sodium sulfide, sodium hydroxide and sublimed sulfur to leach tellurium-containing materials, can realize the efficient separation and extraction of valuable metals such as tellurium, selenium and the like, and enriches heavy metal ions such as copper, lead, bismuth and the like in leaching slag, so that the selective extraction effect is good.
(2) The method adopts the alkaline vulcanization system solution composed of sodium sulfide, sodium hydroxide and sublimed sulfur to leach the tellurium-containing materials, has strong adaptability to raw materials, can treat tellurium-containing materials of different types, and is easy to realize large-scale popularization and application.
(3) According to the invention, sodium sulfite is used as a reducing agent, tellurium and selenium in the leaching solution can be directionally reduced and enriched in an alkaline vulcanization system, and crude tellurium and crude selenium products are prepared in one step, so that the selectivity is good, and the product quality is high; the procedures of purifying, neutralizing, precipitating, calcining, liquid making and the like in the traditional tellurium production process are avoided, the process flow is greatly shortened, and the high-efficiency short-flow clean extraction of tellurium is realized.
(4) The process of the invention is not needed to be carried out under the conditions of high temperature and high pressure, has low energy consumption, simple operation, low requirement on equipment, low cost and easy acquisition of used reagents, low production and investment cost and short factory building period, and can be directly grafted on the traditional tellurium extraction process.
Drawings
Fig. 1 is a flow chart of a process for efficiently separating tellurium and selenium from tellurium-containing materials in example 3 of the present invention.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying drawings, in which preferred embodiments are shown, for the purpose of illustrating the invention, but the scope of the invention is not limited to the specific embodiments shown.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
The various reagents and materials used in the present invention are commercially available or may be prepared by known methods unless otherwise specified.
Example 1:
the copper telluride slag to be treated in this embodiment comprises: 21.71wt% Te, 43.25wt% Cu, 3.23wt% S and 1.29wt% Cl.
The method for efficiently separating tellurium from tellurium-containing materials comprises the following steps:
(1) Sodium sulfide, sublimed sulfur, sodium hydroxide and water are mixed according to a mass ratio of 3:2:3:30, and then reacting for 2 hours at 80 ℃ to obtain an alkaline vulcanization system solution.
(2) Adding copper telluride slag into an alkaline vulcanization system solution for stirring leaching, wherein the excess coefficient of the alkaline vulcanization system solution is 5 times, the leaching temperature is 90 ℃, and the liquid-solid ratio is 5:1, leaching for 3 hours with the ratio unit of mL/g, and filtering after leaching to obtain leaching liquid and leaching slag; in the process, the tellurium leaching rate is 98.55%, while copper is not leached, so that the tellurium is selectively leached.
(3) Adding sodium sulfite into the leaching solution obtained in the step (2) for reduction reaction, wherein the sodium sulfite excess coefficient is 5 times, the reduction temperature is 30 ℃, the reaction is carried out for 3 hours, and after the reaction is finished, the filtration is carried out to obtain tellurium precipitation slag and tellurium precipitation post-liquid; the tellurium precipitation rate in this process was 99.61%.
(4) Carrying out ultrasonic washing on the tellurium precipitation slag obtained in the step (3), washing for 30min at the washing temperature of 30 ℃, and filtering after washing to obtain crude tellurium powder; the main components of the crude tellurium powder comprise 98.77wt% of Te, 0.08wt% of Se, 0.12wt% of Cu, 0.47wt% of S and 0.11wt% of Na.
Comparative example 1:
the copper telluride slag to be treated in this comparative example had the composition: te 21.71wt%, cu 43.25wt%, S3.23 wt%, and Cl 1.29wt% in the same manner as in example 1.
The method for sulfur leaching tellurium from tellurium-containing materials in this comparative example comprises the following steps:
(1) Sodium sulfide, sodium hydroxide and water are mixed according to the mass ratio of 3:3:30, and then reacting for 2 hours at 80 ℃ to obtain a vulcanization system solution.
(2) Adding copper telluride slag into the vulcanizing system solution prepared in the step (1) for stirring leaching, wherein the excess coefficient of the vulcanizing system solution is 5 times, the leaching temperature is 90 ℃, and the liquid-solid ratio is 5:1, leaching for 3 hours with the ratio unit of mL/g, and filtering after leaching to obtain leaching liquid and leaching slag; the leaching rates of tellurium and copper in the process are 74.76% and 1.53%, respectively.
From this, it can be seen that the leaching system composed of sodium sulfide and sodium hydroxide is selected, and the leaching rate of tellurium is not high.
Example 2:
the flotation tailings to be treated in this embodiment are composed of: te 2.03wt%, pb 31.49wt%, sb 7.42wt%, ba 10.03wt%, bi 2.49wt%, S6.45 wt% and C5.87 wt%.
The method for efficiently separating tellurium from tellurium-containing materials comprises the following steps:
(1) Sodium sulfide, sublimed sulfur, sodium hydroxide and water are mixed according to the mass ratio of 2:2:2:40, and reacting at 75 ℃ for 3 hours to obtain an alkaline vulcanization system solution.
(2) Adding the flotation tailings into an alkaline vulcanization system solution for stirring leaching, wherein the excess coefficient of the alkaline vulcanization system solution is 6 times, the leaching temperature is 90 ℃, and the liquid-solid ratio is 7:1, leaching for 2 hours with the ratio unit of mL/g, and filtering after leaching to obtain leaching liquid and leaching slag; in the process, the leaching rates of tellurium and antimony are 95.98 percent and 31.84 percent respectively, while lead and bismuth are not leached.
(3) Adding sodium sulfite into the leaching solution obtained in the step (2) for reduction reaction, wherein the sodium sulfite excess coefficient is 5 times, the reduction temperature is 30 ℃, the reaction is carried out for 3 hours, and after the reaction is finished, the filtration is carried out to obtain tellurium precipitation slag and tellurium precipitation post-liquid; the tellurium precipitation rate in this process was 98.15%.
(4) Carrying out ultrasonic washing on the tellurium precipitation slag obtained in the step (3), wherein the washing temperature is 40 ℃, the washing time is 30min, and filtering after washing to obtain crude tellurium powder; the main components of the crude tellurium powder comprise 97.86wt% of Te, 0.38wt% of S and 1.64wt% of Na.
Comparative example 2:
the flotation tailings to be treated in this comparative example were composed of: te 2.03wt%, pb 31.49wt%, sb 7.42wt%, ba 10.03wt%, bi 2.49wt%, S6.45 wt% and C5.87 wt% in the same manner as in example 2.
The method for leaching tellurium from tellurium-containing materials in this comparative example comprises the following steps:
adding flotation tailings into a leaching agent for stirring leaching, wherein the leaching agent comprises sodium sulfide, sublimed sulfur, sodium hydroxide and water according to the mass ratio of 2:2:2:40, wherein the leaching agent excess coefficient is 6 times, the leaching temperature is 90 ℃, and the liquid-solid ratio is 7:1, leaching for 2 hours with the ratio unit of mL/g, and filtering after leaching to obtain leaching liquid and leaching slag; the tellurium leaching rate in the process is 82.17%.
Therefore, the alkaline vulcanization system prepared by reacting sodium sulfide, sublimed sulfur, sodium hydroxide and water is selected to leach tellurium-containing materials, and compared with other alkaline vulcanization systems, the method can realize high-efficiency separation leaching extraction of tellurium, presumably because sodium sulfide and sublimed sulfur react to generate sodium polysulfide which contains-S-S-bond similar to-O-O-and has certain oxidizing property, so that the leaching effect on tellurium is good.
Example 3:
the tellurium slag to be treated in this embodiment comprises: 15.48wt% of Te, 14.64wt% of Se, 1.15wt% of Cu, 2.36wt% of Ag, 8.80wt% of Pb and 21.67wt% of Na.
The method for efficiently separating tellurium and selenium from tellurium-containing materials in the embodiment is shown in fig. 1, and comprises the following steps:
(1) Sodium sulfide, sublimed sulfur, sodium hydroxide and water are mixed according to a mass ratio of 3:2:3:50, and then reacting for 2 hours at 60 ℃ to obtain an alkaline vulcanization system solution.
(2) Adding tellurium slag into an alkaline vulcanization system solution for stirring leaching, wherein the excess coefficient of the alkaline vulcanization system solution is 5 times, the leaching temperature is 90 ℃, and the liquid-solid ratio is 10:1, leaching for 4 hours with the ratio unit of mL/g, and filtering after stirring leaching to obtain leaching liquid and leaching slag; in the process, the leaching rates of tellurium and selenium are 95.64 percent and 93.63 percent respectively, while copper, lead and silver are not leached.
(3) Adding sodium sulfite into the leaching solution obtained in the step (2) for reduction reaction, wherein the sodium sulfite excess coefficient is 7 times, the reduction temperature is 50 ℃, the reaction is carried out for 4 hours, and filtering is carried out after the reaction is finished to obtain tellurium precipitation slag and tellurium precipitation post-liquid; the precipitation rates of tellurium and selenium in the process are 99.58% and 0.62%, respectively.
(4) Carrying out ultrasonic washing on the tellurium precipitation slag obtained in the step (3) at the temperature of 40 ℃ for 20min, and filtering to obtain crude tellurium powder; the main components of the crude tellurium powder comprise 98.96wt% of Te, 0.19wt% of Se, 0.12wt% of S and 0.09wt% of Na.
(5) Adding hydrogen peroxide into the tellurium precipitation solution obtained in the step (4) for reaction, wherein the hydrogen peroxide excess coefficient is 3, the reaction temperature is 30 ℃, the reaction time is 2 hours, after the oxidation reaction is finished, adding concentrated sulfuric acid with the concentration of 75% to adjust the pH value of the solution to 1, adding sodium sulfite to reduce selenium precipitation, wherein the sodium sulfite excess coefficient is 5 times, the reduction temperature is 40 ℃, the reduction time is 4 hours, and filtering after the reaction is finished to obtain selenium precipitation slag and selenium precipitation solution; the selenium precipitation rate is 98.96%.
(6) Ultrasonic washing is carried out on the selenium-precipitating slag obtained in the step (5), the washing temperature is 30 ℃, the washing time is 30min, and the crude selenium powder is obtained after washing and filtering; the main component content of the crude selenium powder is 98.79wt% of Se, 0.75wt% of S and 0.42wt% of Na.
Claims (6)
1. A method for efficiently separating tellurium from tellurium-containing materials, comprising the steps of:
(1) Adding tellurium-containing materials into an alkaline vulcanization system solution for leaching, and carrying out solid-liquid separation to obtain tellurium-containing leaching solution and leaching residues; wherein the alkaline vulcanization system solution is a mixed solution prepared from sodium sulfide, sodium hydroxide and sublimed sulfur; the leaching temperature is 70-90 ℃, and the leaching liquid-solid ratio is 5-10: 1, leaching for 2-5 hours, wherein the ratio unit is mL/g; the excess coefficient of the alkaline vulcanization system solution is 5-10 times; the alkaline vulcanization system solution is prepared by mixing the following components in percentage by mass: 1-2: 1-3: mixing 30-50 of sodium sulfide, sublimed sulfur, sodium hydroxide and water, and reacting at 60-80 ℃ for 1-3 hours to obtain a mixed solution;
(2) Adding sodium sulfite into the leaching solution to react, and filtering after the reaction is finished to obtain tellurium precipitation slag and tellurium precipitation post-liquid; washing and filtering the tellurium precipitation slag to obtain crude tellurium powder; the excess coefficient of the sodium sulfite is 3-10 times, the reduction temperature is 30-50 ℃, and the reduction time is 2-5 hours.
2. A method for efficiently separating tellurium and selenium from tellurium-containing materials is characterized by comprising the following steps:
(1) Adding tellurium-containing materials into an alkaline vulcanization system solution for leaching, and carrying out solid-liquid separation to obtain tellurium-containing leaching solution and leaching residues; wherein the alkaline vulcanization system solution is a mixed solution prepared from sodium sulfide, sodium hydroxide and sublimed sulfur; the leaching temperature is 70-90 ℃, and the leaching liquid-solid ratio is 5-10: 1, leaching for 2-5 hours, wherein the ratio unit is mL/g; the excess coefficient of the alkaline vulcanization system solution is 5-10 times; the alkaline vulcanization system solution is prepared by mixing the following components in percentage by mass: 1-2: 1-3: mixing 30-50 of sodium sulfide, sublimed sulfur, sodium hydroxide and water, and reacting at 60-80 ℃ for 1-3 hours to obtain a mixed solution;
(2) Adding sodium sulfite into the leaching solution to react, and filtering after the reaction is finished to obtain tellurium precipitation slag and tellurium precipitation post-liquid; washing and filtering the tellurium precipitation slag to obtain crude tellurium powder; the excess coefficient of the sodium sulfite is 3-10 times, the reduction temperature is 30-50 ℃, and the reduction time is 2-5 hours;
(3) Adding an oxidant into the tellurium precipitation liquid to perform oxidation reaction, adjusting the pH value of the solution to 1-2 after the reaction is finished, adding sodium sulfite to perform the reaction, and filtering after the reaction is finished to obtain selenium precipitation slag and selenium precipitation liquid;
(4) Washing and filtering the selenium-precipitating slag to obtain crude selenium powder.
3. The method according to claim 1 or 2, wherein in the step (2), the sodium sulfite excess factor is 5 to 10 times, the reaction temperature is 30 to 50 ℃, and the reaction time is 2 to 5 hours.
4. The method according to claim 1 or 2, wherein in the step (2), the washing is ultrasonic washing, the washing temperature is 30-50 ℃, and the washing time is 10-30 min.
5. The method of claim 1 or 2, wherein the tellurium-containing material is one or more of copper telluride slag, tellurium slag, flotation tailings.
6. The method of claim 2, wherein in the step (3), the oxidant is hydrogen peroxide, the hydrogen peroxide excess coefficient is 1-3 times, the reaction temperature is 25-35 ℃, and the reaction time is 1-3 hours.
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