CN114920208A - Method for efficiently separating tellurium or tellurium and selenium from tellurium-containing material - Google Patents
Method for efficiently separating tellurium or tellurium and selenium from tellurium-containing material Download PDFInfo
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Abstract
A method for efficiently separating tellurium from a material containing tellurium comprises the following steps: adding the tellurium-containing material into an alkaline vulcanization system solution for leaching, and performing solid-liquid separation to obtain a tellurium-containing leaching solution and leaching residues; wherein the alkaline vulcanization system solution is a mixed solution mainly prepared from sodium sulfide, sodium hydroxide and sublimed sulfur; adding sodium sulfite into the leachate to react to obtain tellurium precipitation slag and a solution after tellurium precipitation; and washing and filtering the tellurium precipitation slag to obtain coarse tellurium powder. Further, the invention also discloses a method for adding an oxidant into the solution after tellurium precipitation for reaction, after the reaction is finished, adjusting the pH value of the solution to 1-2, adding sodium sulfite for reaction, and filtering to obtain selenium precipitation slag and a solution after selenium precipitation; washing the selenium precipitation slag, and filtering to obtain crude selenium powder. The invention adopts the alkaline vulcanization system solution composed of sodium sulfide, sodium hydroxide and sublimed sulfur to leach the tellurium-containing materials, can realize the high-efficiency separation and extraction of valuable metals such as tellurium, selenium and the like, and the heavy metal ions such as copper, lead, bismuth and the like are enriched in the leaching residue, so 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 tellurium and selenium from a material containing tellurium.
Background
Tellurium is a typical rare metal, is known as vitamin of modern industry, national defense and advanced technology, is a supporting raw material of modern high and new technology materials, and is an indispensable key metal for developing new and new industries in strategy of China. Tellurium and its compounds have excellent photoelectric characteristics, and are widely used in solar cells, thermoelectric materials and semiconductor devices, and their demand is increasing.
The tellurium-containing material produced in the copper/lead anode slime oxidation refining process is a main raw material for extracting tellurium, and accounts for more than 90 percent. Due to different anode mud treatment processes of enterprises, tellurium-containing materials are various in types, complex in phase and large in fluctuation of valuable metal content, and can be roughly divided into copper telluride slag, tellurium slag and flotation tailings. The copper telluride slag is mainly from a copper and tellurium removal process in the copper anode slime treatment process, and is produced by the copper anode slime treatment enterprises at present and becomes the most main tellurium extraction raw material. The tellurium slag mainly comes from the pyrogenic process treatment process of copper and lead anode slime and the alkaline refining process of crude bismuth, and the method for recovering tellurium from the tellurium slag mainly comprises an alkaline leaching method, pressurized alkaline leaching, acid leaching, pressurized acid leaching, copper powder replacement, a chlorination method, a solvent extraction method and the like. The flotation tailings are mainly obtained from the process of treating the copper anode slime by a dressing and metallurgy combined process developed by Yunnan copper industry limited company, and the research on 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 recovering tellurium by various large copper and lead smelting enterprises in China at present, sodium tellurite, tellurium dioxide and the like in tellurium slag are leached into a solution by using sodium hydroxide, and a tellurium ingot product (99.99%) is obtained by purifying, removing impurities, precipitating tellurium by neutralization, producing a solution by alkali solution and electrolyzing. The method is mature and stable, and has good product quality, but has poor raw material adaptability (to Na) 2 TeO 3 The tellurium-containing materials mainly have good adaptability, but have poor treatment effect on tellurium-containing materials such as telluride, single substance tellurium and insoluble tellurate), long process flow, low tellurium recovery rate (60-70%), and the like.
The alkaline sulfide leaching is an important hydrometallurgy separation method, is widely applied to efficient separation of tellurium, arsenic, tin and other metals, and has the technical advantages of strong selectivity and high separation efficiency. At present, the method is adopted to remove tellurium-containing solidsThe research on separating and recovering tellurium from the waste is relatively less. The patent publication No. CN104762471A discloses a method for enhanced leaching of tellurium slag, which comprises preparing a solution from two or three of sodium sulfide, sodium sulfite and sodium thiosulfate, adding tellurium slag into the solution at a certain liquid-solid ratio, introducing nitrogen as protective atmosphere, and allowing MeTeO to react at high temperature and high pressure 3 And MeTeO 4 Conversion of insoluble substances to soluble Na 2 TeO 3 And the heavy metal ions in the solution are enabled to generate MeS precipitate, the MeS precipitate enters leaching residues, and finally, the solid-liquid separation is realized by adopting vacuum filtration. The method needs to leach tellurium at high temperature and high pressure, and has the advantages of high energy consumption, complex and dangerous operation and high production cost. Patent publication No. CN106636661A discloses a method for selectively separating and recovering tellurium from tellurium slag, in which the tellurium slag is added to a sodium sulfide solution, stirred and leached, and then sodium sulfite is added to the obtained leachate to reduce the solution to obtain crude tellurium. Although the method has good separation effect, high selectivity and simple process, the raw material adaptability is poor, and the method is not suitable for treating tellurium-containing materials such as copper telluride slag, flotation tailings and the like.
In summary, the anode slime treatment processes are different, so that the tellurium-containing materials are various in variety, and the prior treatment process cannot realize the centralized treatment of different types of tellurium-containing materials, so that the production scale of tellurium is small, and the stable supply to the upstream market cannot be met. Therefore, it is urgently needed to develop a method for efficiently separating tellurium in different types of tellurium-containing materials, which has strong raw material adaptability and is easy to popularize and apply in a large scale.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for efficiently separating tellurium from a tellurium-containing material or 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 a tellurium-containing material comprises the following steps:
(1) adding the tellurium-containing material into an alkaline vulcanization system solution for leaching, and performing solid-liquid separation to obtain a 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 leachate to react, and filtering after the reaction is finished to obtain tellurium precipitation slag and a solution after tellurium precipitation; washing and filtering the tellurium precipitation slag to obtain coarse tellurium powder.
As a general inventive concept, the present invention also provides a method for efficiently separating tellurium and selenium from a tellurium-containing material, comprising the steps of:
(1) adding the tellurium-containing material into an alkaline vulcanization system solution for leaching, and performing solid-liquid separation to obtain a 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 leachate for reaction, and filtering after the reaction is finished to obtain tellurium precipitation slag and a solution after tellurium precipitation; washing and filtering the tellurium precipitation slag to obtain coarse tellurium powder;
(3) adding an oxidant into the tellurium-precipitated solution for oxidation reaction, after the reaction is finished, adjusting the pH value of the solution to 1-2, adding sodium sulfite for reaction, and filtering after the reaction is finished to obtain selenium-precipitated slag and selenium-precipitated solution;
(4) washing the selenium precipitation slag, and filtering to obtain crude selenium powder.
Preferably, in the method, in the step (1), the leaching temperature is 70-90 ℃, and the solid-to-solid ratio of the leaching solution is 5-10: 1, the specific value unit is mL/g, and the leaching time is 2-5 h.
In the method, preferably, in the step (1), the excess coefficient of the alkaline vulcanization system solution is 5-10 times. The excessive alkaline sulfide system solution is in the range, the leaching effect of selenium and tellurium is optimal, and the leaching rate of heavy metal ions such as copper is low.
In the method, preferably, in the step (1), the alkaline vulcanization system solution is prepared by mixing, by mass, 1-3: 1-2: 1-3: and (3) mixing 30-50 parts of sodium sulfide, sublimed sulfur, sodium hydroxide and water, and reacting at 60-80 ℃ for 1-3 hours to obtain a mixed solution.
Complex ionic composition (S) in alkaline vulcanization system 2- 、S a 2- 、S 2 O 3 2- ) When the material containing tellurium is added into the alkaline vulcanization system, the sodium tellurite, the tellurium oxide and the tellurium oxide will react with S 2- 、S a 2- 、S 2 O 3 2- Plasma reacting to transform into Te (VI) S x O y 2- And Te (IV) S x O y 2- And leaching, wherein heavy metal ions such as Cu are precipitated in a form of MeS and stored in leaching slag, so that selective extraction of tellurium is realized. 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)
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.
Preferably, in the step (2) and the step (4), the washing is ultrasonic washing, the washing temperature is 30-50 ℃, and the washing time is 10-30 min. The tellurium precipitation slag and the selenium precipitation slag obtained by directional reduction in an alkaline vulcanization system contain a large amount of sulfur and sodium, which affect the product quality, and the sulfur and sodium impurities in the product can be completely removed after ultrasonic washing, so that the crude tellurium powder and the crude selenium powder with higher purity can be 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 phases of the copper telluride slag are CuO and Cu 2 O、Cu 5 Te 3 、Cu 2 Te, the main chemical components are Te, Cu, S and Cl; the main phase in flotation tailings is PbSO 4 、BaSO 4 、TeO 2 、PbSbO 6 The main chemical components are Te, Pb, Sb, Ba, Bi, S and C; the main phase in the tellurium slag is Te 2 O 5 、Na 2 SeO 4 、Na 4 PbO 4 The main chemical components are Te, Se, Cu, Ag, Pb and Na.
In the above method, preferably, in the step (3), the oxidant is hydrogen peroxide, the excess coefficient of hydrogen peroxide is 1-3 times, the reaction temperature is 25-35 ℃, and the reaction time is 1-3 hours.
In the 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 invention adopts the alkaline vulcanization system solution composed of sodium sulfide, sodium hydroxide and sublimed sulfur to leach the tellurium-containing materials, can realize the high-efficiency separation and extraction of valuable metals such as tellurium, selenium and the like, and the heavy metal ions such as copper, lead, bismuth and the like are enriched in the leaching residue, so the selective extraction effect is good.
(2) The method adopts the alkaline vulcanization system solution consisting of the sodium sulfide, the sodium hydroxide and the sublimed sulfur to leach the tellurium-containing materials, has strong adaptability to raw materials, can treat different types of tellurium-containing materials, 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 leachate can be directionally reduced and enriched in an alkaline vulcanization system, crude tellurium and crude selenium products are obtained by one-step preparation, the selectivity is good, and the product quality is high; the processes of purification, neutralization, precipitation, calcination, liquid making and the like in the traditional tellurium production process are avoided, the process flow is greatly shortened, and the efficient short-flow clean extraction of tellurium is realized.
(4) The process of the invention does not need to be carried out under the conditions of high temperature and high pressure, has low energy consumption, simple and convenient operation, low requirement on equipment, cheap and easily-obtained used reagents, low production and investment cost and short plant building period, and can be directly grafted to the traditional tellurium extraction process.
Drawings
Fig. 1 is a process flow chart of the process for efficiently separating tellurium and selenium from a tellurium-containing material in example 3 of the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art 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 limit the scope of the present invention.
Unless otherwise specified, the reagents and materials used in the present invention are commercially available products or products produced by known methods.
Example 1:
the copper telluride slag to be treated in the embodiment comprises the following components: te 21.71 wt%, Cu 43.25 wt%, S3.23 wt%, Cl 1.29 wt%.
The method for efficiently separating tellurium from the tellurium-containing material comprises the following steps:
(1) mixing sodium sulfide, sublimed sulfur, sodium hydroxide and water 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 the copper telluride slag into an alkaline vulcanization system solution for agitation 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 specific value unit of mL/g, and filtering after leaching to obtain leachate and leaching residues; in the process, the tellurium leaching rate is 98.55 percent, and the copper is not leached, so that the selective leaching of tellurium is realized.
(3) Adding sodium sulfite into the leachate obtained in the step (2) to carry out reduction reaction, wherein the excess coefficient of the sodium sulfite is 5 times, the reduction temperature is 30 ℃, reacting for 3 hours, and filtering after the reaction is finished to obtain tellurium precipitation slag and a liquid after the tellurium precipitation; the precipitation rate of tellurium in this process was 99.61%.
(4) Carrying out ultrasonic washing on the tellurium precipitation slag obtained in the step (3), wherein the washing temperature is 30 ℃, washing for 30min, and filtering after washing to obtain crude tellurium powder; the main component contents of the coarse tellurium powder are 98.77 wt% of Te, 0.08 wt% of Se, 0.12 wt% of Cu, 0.47 wt% of S and 0.11 wt% of Na.
Comparative example 1:
the copper telluride slag to be treated in the comparative example comprises the following components: te 21.71 wt%, Cu 43.25 wt%, S3.23 wt%, and Cl 1.29 wt% were the same as in example 1.
The method for sulfide leaching of tellurium from the tellurium-containing material comprises the following steps:
(1) mixing sodium sulfide, sodium hydroxide and water 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 the copper telluride slag into the vulcanization system solution prepared in the step (1) for stirring leaching, wherein the excess coefficient of the 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 specific value unit of mL/g, and filtering after leaching to obtain leachate and leaching residues; the leaching rates of tellurium and copper in the process are respectively 74.76 percent and 1.53 percent.
Therefore, the leaching system consisting of sodium sulfide and sodium hydroxide is not high in tellurium leaching rate.
Example 2:
the flotation tailings to be treated in this example consist of: te 2.03 wt%, Pb 31.49 wt%, Sb 7.42 wt%, Ba 10.03 wt%, Bi 2.49 wt%, S6.45 wt%, C5.87 wt%.
The method for efficiently separating tellurium from the tellurium-containing material comprises the following steps:
(1) mixing sodium sulfide, sublimed sulfur, sodium hydroxide and water according to a mass ratio of 2: 2: 2: 40, and reacting for 3 hours at 75 ℃ to obtain an alkaline vulcanization system solution.
(2) Adding the flotation tailings into an alkaline vulcanization system solution, stirring and 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 specific value unit of mL/g, and filtering after leaching to obtain a leaching solution and leaching residues; in the process, the leaching rates of tellurium and antimony are 95.98% and 31.84%, respectively, and lead and bismuth are not leached.
(3) Adding sodium sulfite into the leachate obtained in the step (2) to carry out reduction reaction, wherein the excess coefficient of the sodium sulfite is 5 times, the reduction temperature is 30 ℃, reacting for 3 hours, and filtering after the reaction is finished to obtain tellurium precipitation slag and a liquid after the tellurium precipitation; the precipitation rate of tellurium 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 coarse tellurium powder are 97.86 wt% of Te, 0.38 wt% of S and 1.64 wt% of Na.
Comparative example 2:
the flotation tailings to be treated in the comparative example consist of: te 2.03 wt%, Pb 31.49 wt%, Sb 7.42 wt%, Ba 10.03 wt%, Bi 2.49 wt%, S6.45 wt%, C5.87 wt%, and the same as in example 2.
The method for leaching tellurium from the material containing tellurium in the comparative example comprises the following steps:
adding the flotation tailings into a leaching agent for agitation leaching, wherein the leaching agent is prepared from sodium sulfide, sublimed sulfur, sodium hydroxide and water in a mass ratio of 2: 2: 2: 40, the excess coefficient of the leaching agent is 6 times, the leaching temperature is 90 ℃, and the liquid-solid ratio is 7: 1, leaching for 2 hours with the specific value unit of mL/g, and filtering after leaching to obtain a leaching solution and leaching residues; 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 the tellurium-containing material, and compared with other alkaline vulcanization systems, efficient separation, leaching and extraction of tellurium can be realized.
Example 3:
the tellurium slag to be treated in this example consists of: 15.48 wt% of Te, 14.64 wt% of Se, 1.15 wt% of Cu, 2.36 wt% of Ag, 8.80 wt% of Pb and 21.67 wt% of Na.
The process flow diagram of the method for efficiently separating tellurium and selenium from a material containing tellurium is shown in fig. 1, and the method comprises the following steps:
(1) mixing sodium sulfide, sublimed sulfur, sodium hydroxide and water 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, stirring and 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 specific value unit of mL/g, and filtering after stirring and leaching to obtain leachate and leaching residues; in the process, the leaching rates of tellurium and selenium are 95.64% and 93.63%, respectively, while copper, lead and silver are not leached.
(3) Adding sodium sulfite into the leachate obtained in the step (2) to carry out reduction reaction, wherein the excess coefficient of the sodium sulfite is 7 times, the reduction temperature is 50 ℃, reacting for 4 hours, and filtering after the reaction is finished to obtain tellurium precipitation slag and a liquid after the tellurium precipitation; the precipitation rates of tellurium and selenium in the process were 99.58% and 0.62%, respectively.
(4) Ultrasonically washing the tellurium precipitation slag obtained in the step (3) at the temperature of 40 ℃, washing for 20min, and filtering to obtain coarse tellurium powder; the main components of the coarse tellurium powder comprise 98.96 wt% of Te, 0.19 wt% of Se, 0.12 wt% of S and 0.09 wt% of Na.
(5) Adding hydrogen peroxide into the tellurium-precipitated liquid obtained in the step (4) for reaction, wherein the excess coefficient of the hydrogen peroxide is 3, the reaction temperature is 30 ℃, the reaction time is 2h, 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 and precipitate selenium, the excess coefficient of the sodium sulfite is 5 times, the reduction temperature is 40 ℃, the reduction time is 4h, and filtering after the reaction is finished to obtain selenium-precipitated slag and selenium-precipitated liquid; the selenium precipitation rate was 98.96%.
(6) Ultrasonically washing the selenium precipitation slag obtained in the step (5), wherein the washing temperature is 30 ℃, the washing time is 30min, and filtering after washing to obtain crude selenium powder; the content of main components in the crude selenium powder is 98.79wt percent of Se, 0.75wt percent of S and 0.42wt percent of Na.
Claims (10)
1. A method for efficiently separating tellurium from a tellurium-containing material is characterized by comprising the following steps:
(1) adding the tellurium-containing material into an alkaline vulcanization system solution for leaching, and performing solid-liquid separation to obtain a tellurium-containing leaching solution and leaching residues; wherein the alkaline vulcanization system solution is a mixed solution mainly prepared from sodium sulfide, sodium hydroxide and sublimed sulfur;
(2) adding sodium sulfite into the leachate for reaction, and filtering after the reaction is finished to obtain tellurium precipitation slag and a solution after tellurium precipitation; and washing and filtering the tellurium precipitation slag to obtain coarse tellurium powder.
2. A method for efficiently separating tellurium and selenium from a tellurium-containing material is characterized by comprising the following steps:
(1) adding the tellurium-containing material into an alkaline vulcanization system solution for leaching, and performing solid-liquid separation to obtain a tellurium-containing leaching solution and leaching residues; wherein the alkaline vulcanization system solution is a mixed solution mainly prepared from sodium sulfide, sodium hydroxide and sublimed sulfur;
(2) adding sodium sulfite into the leachate for reaction, and filtering after the reaction is finished to obtain tellurium precipitation slag and a solution after tellurium precipitation; washing and filtering the tellurium precipitation slag to obtain coarse tellurium powder;
(3) adding an oxidant into the solution after tellurium precipitation 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 a solution after selenium precipitation;
(4) washing the selenium precipitation slag, and filtering to obtain crude selenium powder.
3. The method of claim 1 or 2, wherein in the step (1), the leaching temperature is 70-90 ℃, and the leaching liquid-solid ratio is 5-10: 1, the unit of the ratio is mL/g, and the leaching time is 2-5 h.
4. The method of claim 1 or 2, wherein in step (1), the alkaline vulcanization system solution has an excess factor of 5 to 10 times.
5. The method according to claim 1 or 2, wherein in the step (1), the alkaline vulcanization system solution is prepared by mixing the components in a mass ratio of 1-3: 1-2: 1-3: and (3) mixing 30-50 parts of sodium sulfide, sublimed sulfur, sodium hydroxide and water, and reacting at 60-80 ℃ for 1-3 hours to obtain a mixed solution.
6. The method of claim 1 or 2, wherein 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 h.
7. 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.
8. The method of claim 1 or 2, wherein the tellurium-containing material is one or more of copper telluride slag, tellurium slag, flotation tailings.
9. The method as claimed in claim 2, wherein in the step (3), the oxidant is hydrogen peroxide, the excess coefficient of hydrogen peroxide is 1-3 times, the reaction temperature is 25-35 ℃, and the reaction time is 1-3 h.
10. The method of claim 2, wherein the sodium sulfite has an excess coefficient of 3 to 10 times, a reduction temperature of 30 to 50 ℃, and a reduction time of 2 to 5 hours.
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