CN109231175A - A method of impure selenium is purified with dehydrated alcohol - Google Patents
A method of impure selenium is purified with dehydrated alcohol Download PDFInfo
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- CN109231175A CN109231175A CN201811352997.1A CN201811352997A CN109231175A CN 109231175 A CN109231175 A CN 109231175A CN 201811352997 A CN201811352997 A CN 201811352997A CN 109231175 A CN109231175 A CN 109231175A
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- Prior art keywords
- selenium
- dehydrated alcohol
- impure
- sodium thiosulfate
- precipitating
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- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 239000011669 selenium Substances 0.000 title claims abstract description 88
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229960000935 dehydrated alcohol Drugs 0.000 title claims abstract description 21
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims abstract description 27
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims abstract description 16
- 235000019345 sodium thiosulphate Nutrition 0.000 claims abstract description 16
- 238000000746 purification Methods 0.000 claims abstract description 13
- 235000010265 sodium sulphite Nutrition 0.000 claims abstract description 13
- 230000001376 precipitating effect Effects 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 229910052802 copper Inorganic materials 0.000 abstract description 4
- 239000010949 copper Substances 0.000 abstract description 4
- 238000000605 extraction Methods 0.000 abstract description 4
- 238000002386 leaching Methods 0.000 abstract description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052709 silver Inorganic materials 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052737 gold Inorganic materials 0.000 abstract description 2
- 239000010931 gold Substances 0.000 abstract description 2
- 238000009854 hydrometallurgy Methods 0.000 abstract description 2
- 239000004332 silver Substances 0.000 abstract description 2
- 239000011133 lead Substances 0.000 abstract 1
- 229910052714 tellurium Inorganic materials 0.000 abstract 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000005292 vacuum distillation Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910000058 selane Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 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
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- XYUNNDAEUQFHGV-UHFFFAOYSA-N [Se].[Se] Chemical compound [Se].[Se] XYUNNDAEUQFHGV-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 229940127089 cytotoxic agent Drugs 0.000 description 1
- 239000002254 cytotoxic agent Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000014106 fortified food Nutrition 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 239000003978 infusion fluid Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 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
- 239000000049 pigment Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004857 zone melting 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a kind of method with dehydrated alcohol purification impure selenium, belongs to hydrometallurgy field of engineering technology.The method of the invention is leached impure selenium (containing selenium 90% ~ 99%) using sodium sulfite solution, and extraction temperature is 50~150 DEG C, and extraction time is 0.5~3h, and mixing speed is 100~350r/min.Sodium thiosulfate leachate is obtained by filtration after leaching, obtained sodium thiosulfate leachate and excessive dehydrated alcohol are mixed to obtain selenium precipitating, last selenium precipitating obtains the smart selenium that purity is 99.99% ~ 99.999% after washing, filtering, drying.The metal impurities such as tellurium, lead, copper, silver, gold in leached mud are further enriched with.Selenium is precipitated from sodium thiosulfate solution using dehydrated alcohol in the present invention, to realize the high efficiency extraction and purification of selenium, whole process does not have exhaust gas, waste residue to generate.
Description
Technical field
The present invention relates to a kind of methods with dehydrated alcohol purification impure selenium, belong to hydrometallurgy field of engineering technology.
Technical background
Selenium is dissipated metal, and the critical role in national economy and human health is more and more prominent.Selenium has widely
Application field is mainly used for electronics industry such as photoelectric tube, solar battery, pigment industry.In terms of human health, selenium is human body
One of required microelement, selenium-enriched food also receives extensive concern, also functions to key effect in the synthesis of human cytotoxic drug.
The production of high-purity selenium is also paid much attention to；For a long time, the selenium of China's production is mainly that the technical grade of 98% or more purity produces
Product seriously limit the exploitation of high-tech new material, and the selenium of higher purity is dependent on external a large amount of imports.
There is 90% selenium mainly to recycle and obtain from the copper electrolyzing refining earth of positive pole earth of positive pole in the world at present, but is often associated with
There are many impurity such as Te, Pb, Cu, Ag, S, needs further to purify.At present according to purification principle, the method for purification of selenium is mainly divided
For physical purification and chemical purification two major classes.Physical method has vacuum distillation method, zone melting method etc..Vacuum distillation method can efficiently divide
From the high-melting-points such as copper, silver, gold, low saturated vapour pressure impurity, but reduced levels are difficult to remove for impurity such as Te, Pb, S；Area
Domain smelting process is a kind of effective ways purified metals, but the production cycle is longer, is not suitable for large-scale production.Chemical method has impure selenium
Voloxidation-sulfur dioxide reduction method, hydrogen selenide thermal decomposition method, Arbiso process and solvent extraction and ion-exchange etc.；
Oxygen volatilization-sulfur dioxide reduction method experimental condition is more demanding, and process flow is complicated, and working condition is poor, pollutes environment；Selenizing
Hypertoxic gas hydrogen selenide can be generated during hydrogen thermal decomposition method purification selenium, institute in this way only can a small amount of high purity selenium.Sulfurous
Sour sodium method can effectively remove the impurity that vacuum distillation method is difficult to remove, and this method is the sodium sulfite solution that heat is dissolved in using selenium
In and impurity is insoluble, selenium infusion solution by filtering, be precipitated selenium after crystallisation by cooling naturally, but natural precipitation process exist it is time-consuming
Long, the disadvantages of rate of recovery is extremely low.Compared with the method for purification of selenium is precipitated naturally in traditional handicraft sodium sulfite solution leaching-, this hair
The bright precipitation for promoting selenium using dehydrated alcohol, can be obviously shortened the precipitation time of selenium, greatly improve smart selenium recovery.
Summary of the invention
The present invention provides a kind of methods with dehydrated alcohol purification impure selenium, can obtain the higher smart selenium of purity, and mistake
Journey is simple, not can cause environmental pollution without waste water generation, and cost is lower, specifically includes the following steps:
(1) impure selenium raw material is dissolved in sodium sulfite solution, sodium thiosulfate leachate is obtained by filtration after agitating and heating；
(2) at normal temperature, obtained sodium thiosulfate leachate and dehydrated alcohol are mixed to be precipitated and obtain selenium precipitating；
(3) selenium precipitating is filtered, washed, is dried to obtain the smart selenium that purity is 99.99% ~ 99.999%.
Preferably, the selenium powder that impure selenium material purity of the present invention is 90% ~ 99%, selenium powder cross 50 meshes.
Preferably, the concentration of sodium sulfite solution of the present invention is that 300g/L, sodium sulfite solution and impure selenium are solid by liquid
Than for (5 ~ 20): 1 ratio is added in reaction kettle simultaneously；Heating temperature is 50~150 DEG C, 0.5~3h of heating time, stirring speed
Degree is 100~350r/min.
Preferably, the volume of dehydrated alcohol of the present invention is greater than the volume of sodium thiosulfate leachate.
Preferably, filtering of the present invention needs twice, and drying temperature is 60 DEG C.
Leachate first is obtained to impure selenium feedstock purification using Arbiso process in the present invention, sodium sulfite solution dissolution is thick
Selenium is wet process reaction, and the main chemical reactions of generation are as follows:
Se(s) + Na2SO3(aq) = Na2SeSO3(aq)
Beneficial effects of the present invention:
The present invention not only promotes selenium using dehydrated alcohol and is precipitated from sodium thiosulfate solution, but also realizes the high efficiency extraction of selenium
With purification, whole process does not have exhaust gas, waste residue to generate, and waste liquid, which can evaporate to isolate dehydrated alcohol and continue Returning process, to be used for from selenium
Selenium is extracted in sodium thiosulfate solution, finally obtains to obtain the smart selenium that purity is 99.99% ~ 99.999%.
Detailed description of the invention
Fig. 1 is flow diagram of the invention.
Specific embodiment
Below in conjunction with the embodiment in the present invention, clear, complete description is carried out to technical solution of the present invention, but send out
Bright protection scope is not limited to the content.
Embodiment 1
A method of impure selenium being purified with dehydrated alcohol, specifically includes the following steps:
Impure selenium raw material is crushed, crosses 50 meshes, the sodium sulfite solution 300ml and purity for then preparing 300g/L are 90%
Impure selenium raw material by liquid-solid ratio be 15:1 simultaneously be added in reaction kettle, controlled at 120 DEG C, mixing speed 350r/min,
3h is reacted under oil bath heating, magnetic agitation, leachate containing selenium is obtained by filtration.
It measures excessive dehydrated alcohol with graduated cylinder to be added in sodium thiosulfate leachate, low whipping speed 320r/min
Under conditions of be instantly available selenium precipitating, selenium precipitating is using obtaining smart selenium after being filtered, washed, drying (60 DEG C)；The Chinese referring in
The people republic non-ferrous metal industry standard YS/T223-2007 and YS/T226.13-2009, using inductively coupled plasma constitution
Spectrometer (ICP-MS) detects the purity of smart selenium.The purity of smart selenium is 99.991%, and the leaching rate of selenium is 97.53%, comprehensive
Direct yield is 94.3562%.
Table 1: 1 impure selenium of embodiment (Se 90%) purifies result
Embodiment 2
A method of impure selenium being purified with dehydrated alcohol, specifically includes the following steps:
Impure selenium raw material is crushed, crosses 50 meshes, the sodium sulfite solution 300ml and purity for preparing 300g/L are 93% impure selenium
Raw material is that 20:1 is added in reacting furnace simultaneously by liquid-solid ratio, and controlled at 110 DEG C, mixing speed 300r/min, machinery is stirred
Lower reaction 2h is mixed, sodium thiosulfate leachate is obtained by filtration.
It is added in sodium thiosulfate leachate with the excessive dehydrated alcohol of graduated cylinder measurement and obtains selenium precipitating, selenium precipitating passes through again
Be filtered, washed, dry (60 DEG C) after obtain smart selenium；Obtained smart selenium is referring to People's Republic of China's non-ferrous metal industry standard
YS/T223-2007 and YS/T226.13-2009, using icp ms (ICP-MS) to the purity of smart selenium
It is detected.The purity of smart selenium is 99.993%, and the leaching rate of selenium is 97.63%, and comprehensive direct yield is 94.65%.
Table 2: 2 impure selenium of embodiment (Se 93%) purifies result
Embodiment 3
A method of impure selenium being purified with dehydrated alcohol, specifically includes the following steps:
Impure selenium raw material is crushed, crosses 50 meshes, impure selenium raw material is handled, the sodium sulfite solution of 300g/L is prepared
It by liquid-solid ratio is that 9:1 is added in reacting furnace simultaneously that 300ml and purity, which are 99% impure selenium raw material, controlled at 50 DEG C, mixing speed
For 200r/min, 1.5h is reacted under mechanical stirring, sodium thiosulfate leachate is obtained by filtration.
It is added in sodium thiosulfate leachate with the excessive dehydrated alcohol of graduated cylinder measurement and obtains selenium precipitating, selenium precipitating passes through again
Be filtered, washed, dry (60 DEG C) after obtain smart selenium；Obtained smart selenium is referring to People's Republic of China's non-ferrous metal industry standard
YS/T223-2007 and YS/T226.13-2009, using icp ms (ICP-MS) to the purity of smart selenium
It is detected.The purity of smart selenium is 99.9990%, and the leaching rate of selenium is 97.6324%, and comprehensive direct yield is 94.6522%.
Table 3: 3 impure selenium of embodiment (Se 99%) purifies result
Claims (5)
1. a kind of method with dehydrated alcohol purification impure selenium, which is characterized in that specifically includes the following steps:
(1) impure selenium raw material is dissolved in sodium sulfite solution, sodium thiosulfate leachate is obtained by filtration after agitating and heating；
(2) at normal temperature, obtained sodium thiosulfate leachate and dehydrated alcohol are mixed to be precipitated and obtain selenium precipitating；
(3) selenium precipitating is filtered, washed, is dried to obtain smart selenium.
2. method according to claim 1, it is characterised in that: the selenium powder that impure selenium material purity is 90% ~ 99%, selenium powder cross 50 mesh
Sieve.
3. method according to claim 1, it is characterised in that: the concentration of sodium sulfite solution is 300g/L, and sodium sulfite is molten
Liquid and impure selenium are (5 ~ 20) in liquid-solid ratio: 1 ratio is added in reaction kettle simultaneously；Heating temperature is 50~150 DEG C, heating time
0.5~3h, mixing speed are 100~350r/min.
4. method according to claim 1, it is characterised in that: the volume of dehydrated alcohol is greater than the body of sodium thiosulfate leachate
Product.
5. method according to claim 1, which is characterized in that filtering needs twice, and drying temperature is 60 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811352997.1A CN109231175A (en) | 2018-11-14 | 2018-11-14 | A method of impure selenium is purified with dehydrated alcohol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811352997.1A CN109231175A (en) | 2018-11-14 | 2018-11-14 | A method of impure selenium is purified with dehydrated alcohol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109231175A true CN109231175A (en) | 2019-01-18 |
Family
ID=65074665
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811352997.1A Pending CN109231175A (en) | 2018-11-14 | 2018-11-14 | A method of impure selenium is purified with dehydrated alcohol |
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| Country | Link |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109911869A (en) * | 2019-03-12 | 2019-06-21 | 湖南工业大学 | A kind of method that selenium is extracted in the cleaning of selenic acid scum reduction decomposition |
| CN110668471A (en) * | 2019-10-22 | 2020-01-10 | 成都市科隆化学品有限公司 | Purification production method of environment-friendly potassium persulfate |
| CN111517290A (en) * | 2020-05-12 | 2020-08-11 | 昆明冶金研究院有限公司 | Method for preparing refined selenium by two-step method |
| CN111689479A (en) * | 2020-07-01 | 2020-09-22 | 昆明冶金研究院有限公司 | Medicament SC-500 for removing As, Pb and Sb and preparation method and application thereof |
| CN112125284A (en) * | 2020-08-31 | 2020-12-25 | 河南师范大学 | Preparation method and medical application of amorphous nano-selenium with biological activity |
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| US4548800A (en) * | 1982-08-02 | 1985-10-22 | Xerox Corporation | Process for selenium purification |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109911869A (en) * | 2019-03-12 | 2019-06-21 | 湖南工业大学 | A kind of method that selenium is extracted in the cleaning of selenic acid scum reduction decomposition |
| CN110668471A (en) * | 2019-10-22 | 2020-01-10 | 成都市科隆化学品有限公司 | Purification production method of environment-friendly potassium persulfate |
| CN111517290A (en) * | 2020-05-12 | 2020-08-11 | 昆明冶金研究院有限公司 | Method for preparing refined selenium by two-step method |
| CN111689479A (en) * | 2020-07-01 | 2020-09-22 | 昆明冶金研究院有限公司 | Medicament SC-500 for removing As, Pb and Sb and preparation method and application thereof |
| CN112125284A (en) * | 2020-08-31 | 2020-12-25 | 河南师范大学 | Preparation method and medical application of amorphous nano-selenium with biological activity |
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