CN109319746A - A kind of method of vacuum distillation-sodium sulfite combination method purification impure selenium - Google Patents
A kind of method of vacuum distillation-sodium sulfite combination method purification impure selenium Download PDFInfo
- Publication number
- CN109319746A CN109319746A CN201811352990.XA CN201811352990A CN109319746A CN 109319746 A CN109319746 A CN 109319746A CN 201811352990 A CN201811352990 A CN 201811352990A CN 109319746 A CN109319746 A CN 109319746A
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- CN
- China
- Prior art keywords
- selenium
- sodium sulfite
- impure
- vacuum distillation
- impure selenium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000011669 selenium Substances 0.000 title claims abstract description 104
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 98
- 238000000034 method Methods 0.000 title claims abstract description 58
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulphite Substances [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 title claims abstract description 27
- 238000000746 purification Methods 0.000 title claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 235000010265 sodium sulphite Nutrition 0.000 claims abstract description 8
- 230000001376 precipitating effect Effects 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- ZYFVEBWCEZMCBU-UHFFFAOYSA-N selenium;hydrochloride Chemical compound Cl.[Se] ZYFVEBWCEZMCBU-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 238000001556 precipitation Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 14
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 238000010907 mechanical stirring Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 229910000058 selane Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000000049 pigment Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N sulfur dioxide Inorganic materials O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 238000004857 zone melting Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000004291 sulphur dioxide Substances 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 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
Abstract
A kind of method that the present invention discloses vacuum distillation-sodium sulfite combination method purification impure selenium, belongs to impure selenium purification technique field.The method of the invention is that impure selenium raw material is added in vacuum distillation furnace, and the higher impure selenium volatile matter of purity and residue are obtained after heating in vacuum, and residue returns to raw material；Be (5 ~ 10) in liquid-solid ratio: impure selenium volatile matter is dissolved in sodium sulfite solution by 1 ratio, and leachate containing selenium is obtained by filtration after agitating and heating；It is that 5 ~ 6 precipitations are precipitated by obtained leachate containing selenium hydrochloric acid or sulfuric acid regulation solution pH, precipitating is filtered, washed, is dried to obtain smart selenium, and purity is 99.99% ~ 99.999%.The method of the invention can effectively purify selenium, and investment is less, and easy to operate, energy consumption is less, simple production process, and the rate of recovery of smart selenium is greater than 95%.
Description
Technical field
The present invention relates to a kind of vacuum distillation-sodium sulfite combination method purification impure selenium methods, belong to impure selenium purification technique
Field.
Technical background
Selenium is dissipated metal, and as people are to the understanding of selenium and deepening continuously for research, selenium is strong in national economy and the mankind
Critical role in health is more and more prominent.Selenium has a wide range of applications field, is mainly used for electronics industry such as photoelectric tube, solar energy
Battery, pigment industry.Selenium is largely used because pigment containing selenium has stability to light, heat, chemical action.Selenium can also be used to duplicate
Machine, glass decoloration, metallurgical addition agent etc..Therefore the production of high-purity selenium also earns widespread respect.For a long time, the selenium of China's production
The mainly technical grade product of 98% or more purity, the selenium of higher purity is dependent on external a large amount of imports, either still from yield
It is all difficult to meet the development of China's new material in quality.
Recycling, the elemental selenium for extracting acquisition need further to purify containing many impurity.At present according to purification principle, selenium
Method of purification be broadly divided into chemical purification and physical purification two major classes；Chemical method has impure selenium voloxidation-sulphur dioxide reduction
Method, hydrogen selenide thermal decomposition method and solvent extraction and ion-exchange etc.；Oxygen volatilization-sulfur dioxide reduction method experimental condition
More demanding, process flow is complicated, and working condition is poor, pollutes environment；Play can be generated during hydrogen selenide thermal decomposition method purification selenium
Poisonous gas hydrogen selenide, institute in this way only can a small amount of high purity selenium；Physical method has vacuum distillation method, zone melting method etc..Very
The empty way of distillation can efficiently separate the high-melting-points such as copper, silver, gold, low saturated vapour pressure impurity, but the impurity such as tellurium, lead are difficult to remove
To reduced levels；Zone melting method is a kind of effective ways purified metals, but the production cycle is longer, is not suitable for extensive raw
It produces.Conventional process techniques are mature, be easy to control, processing capacity is big, but there are long flow path, metal recovery rate is low, energy consumption is high, pollution
Greatly, the problems such as at high cost.Compared with traditional handicraft, the present invention can shorten the purification process of selenium, improve smart selenium recovery, reduce
Smelt production energy consumption；Meanwhile vacuum distillation-Arbiso process combination method process is simple, environmental-friendly, and cost is lower, smart selenium
Purity it is higher.
Summary of the invention
The purpose of the present invention is to provide a kind of vacuum distillation-sodium sulfite combination method purification impure selenium method, final energy
Enough 99.99% ~ 99.999% smart selenium specifically includes following in addition, method provided by the invention not can cause environmental pollution
Step:
(1) impure selenium raw material is added in vacuum distillation furnace, obtained after heating in vacuum the higher impure selenium volatile matter of purity and
Residue, residue return to raw material.
(2) be (5 ~ 10) in liquid-solid ratio: impure selenium volatile matter is dissolved in sodium sulfite solution by 1 ratio, after agitating and heating
Leachate containing selenium is obtained by filtration.
It (3) is that 5 ~ 6 precipitations are precipitated by obtained leachate containing selenium hydrochloric acid or sulfuric acid regulation solution pH, precipitating is passed through
It filters, wash, being dried to obtain smart selenium.
Preferably, pressure is 1~5Pa in vacuum distillation furnace of the present invention, and vacuum drying oven heating rate is 3 ~ 5 DEG C/min,
Heating temperature is 220~350 DEG C, 60 ~ 120min of soaking time.
Preferably, impure selenium volatile matter of the present invention is dissolved in sodium sulfite solution, and heating temperature is 50~150 DEG C, is added
Hot 0.5~3h of time, mixing speed are 100~350r/min.
Preferably, the hydrochloric acid used in the present invention or sulfuric acid concentration are 3~6mol/L, and adding manner is slowly to drip while stirring
Add.
Preferably, filtering times are that twice, drying temperature is 60 DEG C in step (2) of the present invention.
Preferably, impure selenium raw material used is after drying without containing moisture impure selenium in step (1) of the present invention.
Beneficial effects of the present invention:
Vacuum distillation provided by the invention-sodium sulfite combination method is that the Methods For Purification that is combined using physics and chemical method is thick
Selenium, vacuum distillation, which is both utilized, has the advantages that efficient, cleaning, while efficiently solving single vacuum using Arbiso process and steaming
The method of evaporating is difficult to the shortcomings that removing the impurity such as Te, S, Hg, As, and impure selenium is finally purified to 99.99% ~ 99.999% smart selenium.Entirely
Process is simple, process is short, and cost is lower.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Whole description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments；It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment belongs to, protection scope of the present invention.
Embodiment 1
(1) impure selenium raw material (Se 92%) is added in vacuum distillation furnace, pressure 1Pa, it, will by the heating rate of 3 DEG C/min
Temperature in vacuum distillation furnace is heated to 350 DEG C, and soaking time 120min obtains the higher impure selenium of purity after heating in vacuum and waves
Object and residue are sent out, residue returns to raw material.
(2) impure selenium volatile matter is dissolved in sodium sulfite solution in the ratio that liquid-solid ratio is 10:1, controlled at 50 DEG C,
Mixing speed is 350r/min, reacts 1h under mechanical stirring, leachate containing selenium is obtained by filtration after agitating and heating.
(3) sulfuric acid solution for preparing 3mol/L, it is 6.0 that leachate, which is added, and adjusts pH value of solution, obtains red precipitate, precipitating is again
Smart selenium is obtained after being filtered, washed, drying；The leaching rate of selenium is 95.53%, and final essence selenium direct yield is 96.35%；It obtains
Smart selenium is referring to the People's Republic of China's non-ferrous metal industry standard YS/T223-2007 and YS/T226.13-2009, using inductance
Couple plasma mass spectrometer (ICP-MS) detects the purity of smart selenium；Testing result is shown in Table 1；In the identical situation of condition
Under, individually using vacuum distillation method purification impure selenium, the results are shown in Table 2, individually purifies impure selenium result using Arbiso process
As shown in table 3.
Table 1: 1 impure selenium of embodiment (Se 92%) purifies result
Table 2: impure selenium result is individually purified using vacuum distillation method
Table 3: impure selenium result is individually purified using Arbiso process
Embodiment 2
(1) impure selenium raw material (Se 98%) is added in vacuum distillation furnace, pressure 5Pa, it, will by the heating rate of 4 DEG C/min
Temperature in vacuum distillation furnace is heated to 240 DEG C, and soaking time 90min obtains the higher impure selenium volatilization of purity after heating in vacuum
Object and residue, residue return to raw material.
(2) impure selenium volatile matter is dissolved in sodium sulfite solution in the ratio that liquid-solid ratio is 8:1, controlled at 98 DEG C,
Mixing speed is 100r/min, reacts 2h under mechanical stirring, is obtained by filtration after the agitating and heating of leachate containing selenium to be obtained by filtration and contains
Selenium leachate.
(3) sulfuric acid solution for preparing 3mol/L, it is 5.5 that leachate, which is added, and adjusts pH value of solution, obtains red precipitate, precipitating is again
Smart selenium is obtained after being filtered, washed, drying；The leaching rate of selenium is 96.91%, and final essence selenium direct yield is 95.35%.It obtains
Smart selenium is referring to the People's Republic of China's non-ferrous metal industry standard YS/T223-2007 and YS/T226.13-2009, using inductance
Couple plasma mass spectrometer (ICP-MS) detects the purity of smart selenium；Testing result is shown in Table 4；In the identical situation of condition
Under, individually using vacuum distillation method purification impure selenium, the results are shown in Table 5, individually purifies impure selenium result using Arbiso process
As shown in table 6.
Table 4: 2 impure selenium of embodiment (Se 98%) purifies result
Table 5: impure selenium result is individually purified using vacuum distillation method
Table 6: impure selenium result is individually purified using Arbiso process
Embodiment 3
(1) impure selenium raw material (Se 95%) is added in vacuum distillation furnace, pressure 3Pa, it, will by the heating rate of 5 DEG C/min
Temperature in vacuum distillation furnace is heated to 280 DEG C, and soaking time 90min obtains the higher impure selenium volatilization of purity after heating in vacuum
Object and residue, residue return to raw material.
(2) impure selenium volatile matter is dissolved in sodium sulfite solution in the ratio that liquid-solid ratio is 5:1, controlled at 100 DEG C,
Mixing speed is 300r/min, reacts 3h under mechanical stirring, is obtained by filtration after the agitating and heating of leachate containing selenium to be obtained by filtration and contains
Selenium leachate.
(3) sulfuric acid solution for preparing 3mol/L, it is 5.0 that leachate, which is added, and adjusts pH value of solution, obtains red precipitate, precipitating is again
Smart selenium is obtained after being filtered, washed, drying；The leaching rate of selenium is 98.21%, and final essence selenium direct yield is 97.035%；It obtains
Smart selenium referring to the People's Republic of China's non-ferrous metal industry standard YS/T223-2007 and YS/T226.13-2009, using electricity
Sense couple plasma mass spectrometer (ICP-MS) detects the purity of smart selenium；Testing result is shown in Table 7；In the identical feelings of condition
Under condition, individually using vacuum distillation method purification impure selenium, the results are shown in Table 8, individually purifies impure selenium result using Arbiso process
As shown in table 9.
Table 7: 3 impure selenium of embodiment (Se 95%) purifies result
Table 8: impure selenium result is individually purified using vacuum distillation method
Table 9: impure selenium result is individually purified using Arbiso process
Claims (5)
1. a kind of vacuum distillation-sodium sulfite combination method purification impure selenium method, which comprises the following steps:
(1) impure selenium raw material is added in vacuum distillation furnace, obtained after heating in vacuum the higher impure selenium volatile matter of purity and
Residue, residue return to raw material；
(2) be (5 ~ 10) in liquid-solid ratio: impure selenium volatile matter is dissolved in sodium sulfite solution by 1 ratio, is filtered after agitating and heating
Obtain leachate containing selenium；
(3) be 5 ~ 6 to be precipitated and precipitated by obtained leachate containing selenium hydrochloric acid or sulfuric acid regulation solution pH, precipitating through filtering,
It washs, be dried to obtain smart selenium.
2. vacuum distillation-sodium sulfite combination method purification impure selenium method according to claim 1, it is characterised in that: vacuum
Pressure is 1~5Pa in retort, and vacuum drying oven heating rate is 3 ~ 5 DEG C/min, and heating temperature is 220~350 DEG C, soaking time
60~120min。
3. vacuum distillation-sodium sulfite combination method purification impure selenium method according to claim 1, it is characterised in that: impure selenium
Volatile matter is dissolved in sodium sulfite solution, heating temperature be 50~150 DEG C, 0.5~3h of heating time, mixing speed be 100~
350r/min。
4. vacuum distillation-sodium sulfite combination method purification impure selenium method according to claim 1, it is characterised in that: used
Hydrochloric acid or sulfuric acid concentration be 3~6mol/L, adding manner be slowly added dropwise while stirring.
5. vacuum distillation-sodium sulfite combination method purification impure selenium method according to claim 1, it is characterised in that: step
(2) filtering times are that twice, drying temperature is 60 DEG C in.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811352990.XA CN109319746B (en) | 2018-11-14 | 2018-11-14 | Method for purifying crude selenium by vacuum distillation-sodium sulfite combined method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811352990.XA CN109319746B (en) | 2018-11-14 | 2018-11-14 | Method for purifying crude selenium by vacuum distillation-sodium sulfite combined method |
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| CN109319746B CN109319746B (en) | 2020-05-26 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113353895A (en) * | 2021-08-03 | 2021-09-07 | 金川集团股份有限公司 | Method for extracting crude selenium from selenium-containing material |
| CN113548647A (en) * | 2021-07-16 | 2021-10-26 | 昆明理工大学 | Method for deeply removing arsenic and mercury in crude selenium |
| CN114715859A (en) * | 2022-04-25 | 2022-07-08 | 昆明冶金研究院有限公司 | Method for preparing 3N selenium from selenium slag |
| CN115321492A (en) * | 2022-08-31 | 2022-11-11 | 云南铜业股份有限公司西南铜业分公司 | Method for extracting and purifying selenium under normal pressure |
| 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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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113548647A (en) * | 2021-07-16 | 2021-10-26 | 昆明理工大学 | Method for deeply removing arsenic and mercury in crude selenium |
| CN113353895A (en) * | 2021-08-03 | 2021-09-07 | 金川集团股份有限公司 | Method for extracting crude selenium from selenium-containing material |
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| CN114715859A (en) * | 2022-04-25 | 2022-07-08 | 昆明冶金研究院有限公司 | Method for preparing 3N selenium from selenium slag |
| CN115321492A (en) * | 2022-08-31 | 2022-11-11 | 云南铜业股份有限公司西南铜业分公司 | Method for extracting and purifying selenium under normal pressure |
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