CN110745789A - Crude selenium purification method - Google Patents
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- CN110745789A CN110745789A CN201911058424.2A CN201911058424A CN110745789A CN 110745789 A CN110745789 A CN 110745789A CN 201911058424 A CN201911058424 A CN 201911058424A CN 110745789 A CN110745789 A CN 110745789A
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- selenium
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- 239000011669 selenium Substances 0.000 title claims abstract description 128
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 120
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000000746 purification Methods 0.000 title claims abstract description 7
- 239000002893 slag Substances 0.000 claims abstract description 35
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 25
- 230000001105 regulatory effect Effects 0.000 claims abstract description 24
- 239000012535 impurity Substances 0.000 claims abstract description 21
- 239000011259 mixed solution Substances 0.000 claims abstract description 20
- 239000012065 filter cake Substances 0.000 claims abstract description 19
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000000967 suction filtration Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 43
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 238000004321 preservation Methods 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 230000001276 controlling effect Effects 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 15
- 230000001590 oxidative effect Effects 0.000 abstract description 6
- 239000007800 oxidant agent Substances 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 2
- 239000010949 copper Substances 0.000 description 19
- 229910052802 copper Inorganic materials 0.000 description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 11
- 239000000706 filtrate Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 10
- 229910052714 tellurium Inorganic materials 0.000 description 10
- 239000011133 lead Substances 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 238000004821 distillation Methods 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 238000004448 titration Methods 0.000 description 7
- 238000009833 condensation Methods 0.000 description 6
- 230000005494 condensation Effects 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910018143 SeO3 Inorganic materials 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000005708 Sodium hypochlorite Substances 0.000 description 3
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910018162 SeO2 Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/02—Elemental selenium or tellurium
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a crude selenium purification method, wherein a regulating agent is added into crude selenium slag for size mixing until the pH value is 6.5-7, the regulating agent is used for oxidizing and size mixing the crude selenium slag at the same time, the process period is shortened, the cost is reduced, then, the crude selenium powder is obtained by suction filtration, and the filter cake is condensed after vacuum distillation to obtain refined selenium; adding a regulating agent into the crude selenium slag, wherein the regulating agent is a mixed solution of an oxidant and alkali, and the mixed solution and impurity elements in the crude selenium slag are subjected to oxidation reaction, so that the occurrence state of impurity elements is changed and the pulp is mixed; by utilizing the property difference of the impurity oxide with changed occurrence state and the selenium under the vacuum condition, the selenium and the impurity element are efficiently separated through vacuum distillation, the content of the impurity element in the selenium is reduced, and the selenium product with high purity is obtained.
Description
Technical Field
The invention relates to the field of purification and preparation of rare metals, in particular to a crude selenium purification method.
Technical Field
Selenium, as a rare and dispersive metal, has become a key material for supporting the development of new products of high-tech development and materials (medicines, agriculture and foods). More than 90% of the selenium in industry is produced from the comprehensive recovery and utilization process of the copper anode slime. Copper anode mud is treated by sulfuration roasting, Se is SeO2The gas is volatilized to remove selenium and then is dissolved in water to obtain SeO3 2-Solution, then SO coated2Reducing and precipitating to obtain crude selenium powder; or leaching the copper anode mud by adopting sodium hypochlorite solution to obtain SeO3 2-Solution, then SO coated2Reducing and precipitating to obtain crude selenium powder. The crude selenium powder generally contains more than 65 percent of selenium, more than 20 percent of water, impurity elements such as tellurium, lead, iron, sulfur, rare and precious metal elements and the like, and needs to be purified to produce industrial selenium products. CN1636867 discloses a process for extracting selenium by vacuum smelting, in which a material and a binder are uniformly mixed, dried, granulated, dried to obtain a mixed material, and vacuum distilled to obtain a selenium product, but the purity of the obtained product is not higher than 98%. CN 109336068 discloses a method for removing tellurium from selenium slag to purify selenium, wherein an oxidant is added into crude selenium slag, and the oxidant and tellurium in the crude selenium slag are subjected to oxidation reaction and then are subjected to heating treatment, so that the form of tellurium is changed; tellurium is separated from selenium by vacuum distillation by utilizing the property difference between tellurium oxide with changed form and selenium in vacuum stateRemoving and reducing the tellurium content in the selenium to obtain a selenium product with the purity of more than 99.9 percent. Only the influence of tellurium on the purification of crude selenium is studied, and other impurities are not involved; european rains and the like oxidize selenium in selenium-containing waste into an ionic state by using hydrogen peroxide under a strong acid condition, then add a proper amount of sodium chloride and ammonia water in the reaction process, obtain selenium-containing filtrate through solid-liquid separation, and reduce the selenium-containing filtrate by using hydrazine hydrate to obtain a selenium simple substance, wherein the purity can only reach more than 90%.
Disclosure of Invention
In view of the above, the invention provides a method for purifying crude selenium, which is simple and rapid to operate, does not generate toxic and harmful substances, and has high purity of the obtained refined selenium.
The technical scheme of the invention is as follows:
a method for purifying crude selenium comprises the following steps:
adding a regulating agent into the crude selenium slag for size mixing until the pH value is 6.5-7, oxidizing the crude selenium slag by the regulating agent and carrying out size mixing simultaneously, shortening the process period, reducing the cost, then carrying out suction filtration to obtain filter cake crude selenium powder, and condensing the filter cake crude selenium powder after vacuum distillation to obtain high-purity refined selenium.
The mass fraction of Se in the crude selenium slag is 85-90%, the mass fraction of Te is 1-4%, the mass fraction of Cu is 1-2%, the mass fraction of Pb is 1-2%, and the balance is unavoidable impurities.
The regulating agent is H with the volume ratio of 1: 1-1: 32O2Solution and Na2CO3The mixed solution is formed by mixing solutions or H with the volume ratio of 1: 1-1: 22O2Mixing the solution with NaOH solution to obtain mixed solution; wherein H2O2The mass concentration of the solution is 15 percent, and Na is added2CO3The concentration of the solution is 0.5-1 mol/L, and the concentration of the NaOH solution is 0.5-1 mol/L.
The temperature of the vacuum distillation is 250-280 ℃, the heat preservation time is 1-2 h, and the pressure is 10-200 Pa.
The invention has the beneficial effects that: adding a regulating agent into the crude selenium slag, wherein the regulating agent is a mixed solution of an oxidant and alkali, and the mixed solution and impurity elements in the crude selenium slag are subjected to oxidation reaction, so that the occurrence state of impurity elements is changed and the pulp is mixed; by utilizing the property difference of the impurity oxide with changed occurrence state and the selenium under the vacuum condition, the selenium and the impurity element are efficiently separated through vacuum distillation, the content of the impurity element in the selenium is reduced, and the selenium product with high purity is obtained.
Detailed Description
The invention provides a new process for purifying crude selenium, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A method for purifying crude selenium comprises the following steps:
(1) adding sulfuric acid and water into copper anode slime obtained by copper electrolysis, introducing oxygen to oxidize and remove copper, adding sodium hypochlorite into residues to remove selenium, and obtaining the copper anode slime containing SeO3 2-Introducing SO into the solution2Reducing the obtained crude selenium slag, wherein the mass fraction of Se in the crude selenium slag is 90%, the mass fraction of Te is 1%, the mass fraction of Cu is 1%, the mass fraction of Pb is 2%, and the balance is unavoidable impurities;
(2) putting 50g of the crude selenium slag obtained in the step (1) into a beaker, and slowly adding a regulating agent which is H with the volume ratio of 1:12O2Solution and Na2CO3A mixed solution obtained by mixing the solutions, wherein H2O2The mass concentration of the solution is 15 percent, and Na is added2CO3The concentration of the solution is 1mol/L, the slurry mixing is carried out along with the stirring of a glass rod, the pH value of the mixed material is measured by a pH meter to be 7.00, the adding of the mixed solution is stopped, the solid-liquid mass volume ratio Kg: L of the crude selenium slag to the regulating agent is 0.3:1, the filtering is carried out to obtain 5.6g/L of selenium in the filtrate and obtain a crude selenium filter cake, the crude selenium filter cake is weighed and put into a graphite crucible to be subjected to vacuum distillation treatment, the distillation temperature is 250 ℃, the heat preservation time is 1.5h, the pressure is 10-20 Pa, the selenium product obtained by condensation is prepared by adopting ICP-AES and chemical reaction according to the specification of the Chinese nonferrous metal industry standard YS/T223-2007The purity of the selenium is 99.893% through quantitative analysis of chemical titration; the filtered filtrate and water produced by the vacuum distillation treatment are returned to step (1).
Example 2
A method for purifying crude selenium comprises the following steps:
50g of crude selenium slag is taken and put in a beaker, the mass fraction of Se in the crude selenium slag is 85 percent, the mass fraction of Te is 4 percent, the mass fraction of Cu is 2 percent, the mass fraction of Pb is 2 percent, and the balance is unavoidable impurities, and a regulating agent is slowly added, wherein the regulating agent is H with the volume ratio of 1:22O2Solution and Na2CO3A mixed solution obtained by mixing the solutions, wherein H2O2The mass concentration of the solution is 15 percent, and Na is added2CO3The concentration of the solution is 0.5mol/L, the slurry mixing is carried out along with the stirring of a glass rod, the pH value of the mixed material is measured by a pH meter and is 6.69, the adding of the mixed solution is stopped, the solid-liquid volume ratio Kg: L of the crude selenium slag to the regulating agent is 0.5:1, the filtering is carried out, 3.7g/L of selenium in the filtrate is obtained, a crude selenium filter cake is obtained at the same time, the crude selenium filter cake is weighed, the crude selenium filter cake is placed into a graphite crucible to be subjected to vacuum distillation treatment, the distillation temperature is 270 ℃, the heat preservation time is 1h, the pressure is 50-100 Pa, the selenium product obtained by condensation is quantitatively analyzed by adopting ICP-AES and a chemical titration method according to the stipulation of the Chinese nonferrous metal industry standard YS/T223-2007, and the purity of the selenium.
Example 3
A method for purifying crude selenium comprises the following steps:
putting 50g of crude selenium slag in a beaker, wherein the mass fraction of Se in the crude selenium slag is 88%, the mass fraction of Te is 2%, the mass fraction of Cu is 1.5%, the mass fraction of Pb is 1.5%, and the balance is inevitable impurities, and slowly adding a regulating agent which is H with the volume ratio of 1:32O2Solution and Na2CO3A mixed solution obtained by mixing the solutions, wherein H2O2The mass concentration of the solution is 15 percent, and Na is added2CO3The concentration of the solution is 0.6mol/L, the slurry is mixed with the stirring of the glass rod, the pH value of the mixed material is measured by a pH meter to be 6.92, the adding of the mixed solution is stopped, and at the moment, the crude selenium slag is addedAnd (2) filtering to obtain filtrate containing 1.2g/L of selenium, and simultaneously obtaining a crude selenium filter cake, weighing the crude selenium filter cake, putting the crude selenium filter cake into a graphite crucible to perform vacuum distillation treatment in a vacuum distillation furnace, wherein the distillation temperature is 280 ℃, the heat preservation time is 2 hours, the pressure is 100-200 Pa, and the selenium product obtained by condensation is quantitatively analyzed to have the selenium purity of 99.868 by adopting ICP-AES and a chemical titration method according to the specification of the Chinese nonferrous metal industry standard YS/T223-2007.
Example 4
A method for purifying crude selenium comprises the following steps:
50g of crude selenium slag is taken and put in a beaker, the mass fraction of Se in the crude selenium slag is 90 percent, the mass fraction of Te is 1 percent, the mass fraction of Cu is 1 percent, the mass fraction of Pb is 1 percent, and the balance is unavoidable impurities, and a regulating agent is slowly added, wherein the regulating agent is H with the volume ratio of 1:12O2A mixed solution of the solution and NaOH solution, wherein H is2O2The mass concentration of the solution is 15%, the concentration of the NaOH solution is 1mol/L, the slurry mixing is carried out along with the stirring of a glass rod, the pH value of the mixed material is measured by a pH meter and is 6.50, the addition of the mixed solution is stopped, the solid-liquid mass volume ratio Kg: L of the crude selenium slag to the regulating agent is 0.7:1, the filtering is carried out, the selenium content in the filtrate is 1.2g/L, a crude selenium filter cake is obtained at the same time, the crude selenium filter cake is weighed and is put into a graphite crucible to be subjected to vacuum distillation treatment, the distillation temperature is 250 ℃, the heat preservation time is 2 hours, the pressure is 50-120 Pa, and the selenium product obtained by condensation is quantitatively analyzed by adopting ICP-AES and chemical titration according to the specification of the Chinese nonferrous metal industry standard YS/T223-2007, wherein the purity of the selenium is 99.875%.
Example 5
A method for purifying crude selenium comprises the following steps:
(1) adding sulfuric acid and water into copper anode slime obtained by copper electrolysis, introducing oxygen to oxidize and remove copper, adding sodium hypochlorite into residues to remove selenium, and obtaining the copper anode slime containing SeO3 2-Introducing SO into the solution2The crude selenium slag obtained by reduction comprises 85 mass percent of Se, 4 mass percent of Te, 1 mass percent of Cu, 1 mass percent of Pb and the balance of PbIs inevitable impurity;
(2) putting 50g of the crude selenium slag obtained in the step (1) into a beaker, and slowly adding a regulating agent which is H with the volume ratio of 1:1.52O2A mixed solution of the solution and NaOH solution, wherein H is2O2The mass concentration of the solution is 15%, the concentration of the NaOH solution is 0.5mol/L, the slurry is mixed with the stirring of a glass rod, the pH value of the mixed material is measured by a pH meter to be 7.00, the addition of the mixed solution is stopped, the solid-liquid mass volume ratio Kg: L of the crude selenium slag to the regulating agent is 0.6:1, the filtering is carried out to obtain 1.8g/L of selenium in the filtrate, a crude selenium filter cake is obtained at the same time, the crude selenium filter cake is weighed and put into a graphite crucible to be subjected to vacuum distillation treatment, the distillation temperature is 280 ℃, the heat preservation time is 1h, the pressure is 10-60 Pa, the selenium product obtained by condensation is quantitatively analyzed by adopting ICP-AES and a chemical titration method according to the specification of the Chinese nonferrous metal industry standard YS/T223-2007 to obtain the selenium product with the purity of 99.876%; the filtered filtrate and water produced by the vacuum distillation treatment are returned to step (1).
Example 6
A method for purifying crude selenium comprises the following steps:
50g of crude selenium slag is taken and put in a beaker, the mass fraction of Se in the crude selenium slag is 86 percent, the mass fraction of Te is 3 percent, the mass fraction of Cu is 1.2 percent, the mass fraction of Pb is 1.2 percent, and the balance is inevitable impurities, and a regulating agent is slowly added, wherein the regulating agent is H with the volume ratio of 1:22O2A mixed solution of the solution and NaOH solution, wherein H is2O2The mass concentration of the solution is 15 percent, the concentration of NaOH solution is 1mol/L, the slurry mixing is carried out along with the stirring of ｃA glass rod, the pH value of the mixed material is measured by ｃA pH meter to be 6.00, the adding of the mixed solution is stopped, the solid-liquid mass volume ratio Kg: L of the crude selenium slag to the regulating agent is 0.3:1, the filtering is carried out to obtain the selenium-containing 6.9g/L in the filtrate, ｃA crude selenium filter cake is obtained at the same time, the crude selenium filter cake is weighed, the crude selenium filter cake is put into ｃA graphite crucible to be subjected to vacuum distillation treatment, the distillation temperature is 260 ℃, the heat preservation time is 1.5h, the pressure is 100-200 PｃA, the condensed selenium product is obtained, and the ICP-A method is adopted according to the specification of the Chinese nonferrous metal industry standard YSThe purity of selenium was 99.875% as determined quantitatively by ES and chemical titration.
Comparative example 1
50g of crude selenium slag (the mass percent of Se, 3 percent of Te, 1.2 percent of Cu, 1.2 percent of Pb and the balance of unavoidable impurities in the crude selenium slag) is put into a graphite crucible to be subjected to vacuum distillation treatment, the distillation temperature is 260 ℃, the heat preservation time is 1.5h, the pressure is 100-200 Pa, and the selenium product obtained by condensation is quantitatively analyzed to have the purity of 98.576 percent by adopting ICP-AES and a chemical titration method according to the specification of the Chinese nonferrous metal industry standard YS/T223-2007.
Claims (4)
1. A method for purifying crude selenium is characterized by comprising the following steps:
adding a regulating agent into the crude selenium slag, mixing the slurry until the pH value is 6.5-7, then carrying out suction filtration, and condensing a filter cake after vacuum distillation to obtain refined selenium.
2. The crude selenium purification method according to claim 1, wherein the mass fraction of Se in the crude selenium slag is 85% to 90%, the mass fraction of Te is 1% to 4%, the mass fraction of Cu is 1% to 2%, the mass fraction of Pb is 1% to 2%, and the balance is unavoidable impurities.
3. The method for purifying crude selenium according to claim 1, wherein the controlling agent is H with a volume ratio of 1:1 to 1:32O2Solution and Na2CO3The mixed solution is formed by mixing solutions or H with the volume ratio of 1: 1-1: 22O2Mixing the solution with NaOH solution to obtain mixed solution; wherein H2O2The mass concentration of the solution is 15 percent, and Na is added2CO3The concentration of the solution is 0.5-1 mol/L, and the concentration of the NaOH solution is 0.5-1 mol/L.
4. The method for purifying the crude selenium according to claim 1, wherein the temperature of the vacuum distillation is 250 ℃ to 280 ℃, the heat preservation time is 1 to 2 hours, and the pressure is 10Pa to 200 Pa.
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| CN201911058424.2A CN110745789A (en) | 2019-11-01 | 2019-11-01 | Crude selenium purification method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111977618A (en) * | 2020-08-24 | 2020-11-24 | 昆明理工大学 | Method for removing impurity tellurium from crude selenium powder |
| CN113060708A (en) * | 2021-03-29 | 2021-07-02 | 铜陵有色金属集团股份有限公司 | Production equipment of high-purity selenium and process for preparing high-purity selenium by using production equipment |
| WO2023284332A1 (en) * | 2021-07-16 | 2023-01-19 | 昆明理工大学 | Method for deeply removing arsenic and mercury in crude selenium |
| WO2023142252A1 (en) * | 2022-01-26 | 2023-08-03 | 昆明理工大学 | Apparatus and method for purifying selenium slag in vacuum |
| CN113912024B (en) * | 2021-10-22 | 2024-03-22 | 昆明理工大学 | Method for removing impurity sulfur from selenium-sulfur slag |
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| CN103964402A (en) * | 2013-02-06 | 2014-08-06 | 安徽省思达新材料科技有限公司 | Method for utilizing solid industrial waste containing trace selenium to extract high-purity selenium for new materials |
| CN106853959A (en) * | 2016-09-19 | 2017-06-16 | 三门峡市有色金属质量科学研究所 | A kind of method that use impure selenium wet method prepares high purity selenium |
| CN109336068A (en) * | 2018-12-14 | 2019-02-15 | 昆明鼎邦科技股份有限公司 | The method of tellurium is removed in a kind of impure selenium slag |
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| CN111977618A (en) * | 2020-08-24 | 2020-11-24 | 昆明理工大学 | Method for removing impurity tellurium from crude selenium powder |
| CN111977618B (en) * | 2020-08-24 | 2021-12-07 | 昆明理工大学 | Method for removing impurity tellurium from crude selenium powder |
| CN113060708A (en) * | 2021-03-29 | 2021-07-02 | 铜陵有色金属集团股份有限公司 | Production equipment of high-purity selenium and process for preparing high-purity selenium by using production equipment |
| WO2023284332A1 (en) * | 2021-07-16 | 2023-01-19 | 昆明理工大学 | Method for deeply removing arsenic and mercury in crude selenium |
| CN113912024B (en) * | 2021-10-22 | 2024-03-22 | 昆明理工大学 | Method for removing impurity sulfur from selenium-sulfur slag |
| WO2023142252A1 (en) * | 2022-01-26 | 2023-08-03 | 昆明理工大学 | Apparatus and method for purifying selenium slag in vacuum |
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