CN106868319B - A method of obtaining high purity tellurium from the immersion liquid of alkali containing arsenic - Google Patents
A method of obtaining high purity tellurium from the immersion liquid of alkali containing arsenic Download PDFInfo
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- CN106868319B CN106868319B CN201611192834.2A CN201611192834A CN106868319B CN 106868319 B CN106868319 B CN 106868319B CN 201611192834 A CN201611192834 A CN 201611192834A CN 106868319 B CN106868319 B CN 106868319B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/04—Obtaining arsenic
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
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- 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
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Abstract
A method of high purity tellurium being obtained from the immersion liquid of alkali containing arsenic, the present invention relates to a kind of alkali immersion liquid of the tin of tellurium lead containing arsenic, which is the leachate after oxygen pressure alkali leaching processing high-arsenic antimony flue dust.Alkali immersion liquid is neutralized by sulfuric acid, neutralizer selective reduction, liquid is pure sodium arsenite solution after reduction, is used for the high purity tellurium that the raw material of solution of zinc sulfate arsenic Cobalt Purification nickel, reducing slag and neutralization slag obtain 99.999% or more through hydrogen reduction, vacuum distillation.The present invention will recycle tellurium from high arsenic solution, and obtain pure sodium arsenite solution for zinc hydrometallurgy solution of zinc sulfate arsenic Cobalt Purification nickel raw material.Present invention process flow is short, and the rate of recovery is high, solves pollution problem in traditional handicraft extraction process.
Description
Technical field
The invention belongs to technical field of wet metallurgy, and in particular to the side of high purity tellurium is obtained in a kind of immersion liquid from alkali containing arsenic
Method.
Background technology
Tellurium is widely used in solar cell, optical disc recording, thermoelectric cooling etc., also increasingly by state
The attention and favor of inside and outside scientific worker, tellurium are recognized as one of important support material of 21 century high-technology field.But
It is that tellurium just comes into effect large-scale industrial production in nineteen forty-two, and is quickly grown recently as high technology industry, leads to tellurium
Demand sharply increases.So limited in tellurium reserves, synthetical recovery metal tellurium just has great meaning from waste
Justice.Lead, zinc melting and roasting process in, the high-arsenic antimony flue dust of output not only contains a large amount of arsenic, antimony, also contains a small amount of
Tellurium.After oxygen presses alkali leaching processing high-arsenic antimony flue dust, how the tellurium containing part in the immersion liquid of alkali containing arsenic makes dissipated metal tellurium therein
Synthetical recovery is the problem for failing to solve very well at present.
Chinese invention patent publication number CN103264997A discloses a kind of method for extracting tellurium from low-concentration tellurium solution.
HCl solution is added in low-concentration tellurium solution, obtains pretreatment tellurium liquid water phase, a concentration of 4.5mol/L of wherein HCl；By compared to 1:1
Tributylphosphate/kerosene organic phase is added, 2~4min of oscillation extraction extracts series level-one, and after stratification, obtaining load has
Machine phase；By compared to 1:1 is added NH4Cl solution water phases are stripped, 0.5~2min of oscillation extraction, extract series three-level, are stood and are divided
From water phase；By the water phase containing tellurium after above-mentioned back extraction by evaporation or the precipitation method, tellurium product is made.Invention use extraction → anti-
Extraction → depositing technology flow extracts tellurium from solution containing tellurium, and technological process is long, complicated for operation, while reagent consumption is big.
Chinese invention patent publication number CN101844750A discloses a kind of method of preparing high-purity tellurium by material containing tellurium.It should
Method is that high purity tellurium is prepared using chemical method processing.By materials containing tellurium through peroxidating, acidleach, thick tellurium is obtained by filtration；
The lower acid solution of oxidant effect leaches thick tellurium, through solution containing tellurium is obtained by filtration；Reducing agent is added in solution containing tellurium, after reaction
Reducing agent is added in heating and filtering again in filtrate, and tellurium powder is obtained by filtration after reacting under heating；It is acid under oxidant effect
Reducing agent is added after solution dissolving tellurium powder and obtains smart tellurium；At 200 DEG C~800 DEG C, hydrogen treat essence tellurium obtains high purity tellurium.The hair
The bright smart tellurium technological process of tellurium-contained smelting slag extraction is long, the tediously long complexity of flow, and return period is long.
Invention content
For low, the problem of technological process complexity that solves the tellurium rate of recovery in the immersion liquid of alkali containing tellurium, the present invention propose it is a kind of from containing
The method that high purity tellurium is obtained in arsenic alkali immersion liquid, includes the following steps：
(1) it neutralizes：Take the immersion liquid of alkali containing arsenic, the pH value for adjusting the immersion liquid of alkali containing arsenic is 4-6, after solid-liquor separation, must be neutralized
Liquid and neutralization slag, wherein neutralize slag and enter follow-up hydrogen reduction process；
(2) selective reduction：Reducibility gas is passed through into neutralizer obtained by step (1) to be restored, after reduction,
Reducing solution and reducing slag are obtained after solid-liquor separation；The reducing solution is pure sodium arsenite solution, and it is net to be used as solution of zinc sulfate arsenic
Eliminate the raw material of cobalt nickel；
(3) hydrogen reduction, vacuum distillation：Reducing slag obtained by step (2) carries out hydrogen reduction with neutralization slag obtained by step (1), obtains
To thick tellurium and lead skim, lead skim is as refining leady raw materials, and thick tellurium is in the vacuum distillation furnace of condensation segment and a distilling period there are two having
Vacuum distillation, obtains 99.999% or more high purity tellurium.
The scheme of the invention is being neutralized by sulfuric acid, the tellurium of the lead and a part in alkali immersion liquid, neutralizer selectivity are removed
Reduction, liquid is pure sodium arsenite solution after reduction, is used for the raw material of solution of zinc sulfate arsenic Cobalt Purification nickel, reducing slag and neutralization
Slag obtains 99.999% or more high purity tellurium through hydrogen reduction, vacuum distillation, to realize each valuable metal in the immersion liquid of alkali containing arsenic
Between separation, and have effectively achieved recycling and innoxious.Comprehensive resource utilization rate of the present invention is high, raw material accommodation
Extensively, the pollution problem during traditional extraction technique is solved.
The chemical equation of neutralization step is as follows：
Na2TeO3+H2SO4=TeO2↓+Na2SO4+H2O
Pb2++SO4 2—=PbSO4↓
The sodium tellurite in solution can be transformed into tellurium dioxide to settle down in this way.
The chemical equation for restoring process is as follows：
Na3AsO4+SO2=NaAsO2+Na2SO4
TeOOH++2SO2+2H2O=Te ↓+5H++2SO4 2-
Pb2++SO2+H2O=PbSO3↓+2H+
Pure sodium arsenite solution can be obtained in this way, while being recycled in solution with TeOOH+Existing tellurium.
Then slag and reducing slag will be neutralized again obtains 99.999% high purity tellurium through two processes of hydrogen reduction and vacuum distillation.
This method not only solves the recycling problem of the tellurium in the flue dust of tellurium containing arsenic, and by arsenic recycling.
The immersion liquid of alkali containing arsenic used in the present invention, the leaching for mainly using caustic solution processing arsenic-containing smoke dust to obtain
Liquid.Specifically, the main component of the immersion liquid of alkali containing arsenic be As 1~60g/L, Pb 50ppm~800ppm, Sn 2ppm~
10~120g/L of 200ppm, Te 10~500ppm, NaOH.
Preferably, in step (1), the temperature of neutralization is room temperature to 80 DEG C.
Specifically, the operation of step (1) is：In room temperature to 80 DEG C, mixing speed be 100r/min~300r/min conditions
Under, sour (such as sulfuric acid) is added into the immersion liquid of alkali containing arsenic by solution ph modulation 3~6.
Preferably, in step (2), the reducibility gas is SO2。
Specifically, the operation of step (2) is：Under the conditions of room temperature is to 90 DEG C, according to the speed of 0.5~5L/min, ventilation
0.5~4h.
Preferably, the temperature of hydrogen reduction described in step (3) is controlled at 550 DEG C~650 DEG C.
Preferably, the temperature for two condensation segments being evaporated in vacuo in step (3) is respectively 290 DEG C~310 DEG C and 310 DEG C~
330 DEG C, the temperature of distilling period is controlled at 500 DEG C~550 DEG C.
Preferably, vacuum degree control is 0.1~5Pa in step (3).
The advantages and positive effects of the present invention：
1, the immersion liquid of alkali containing arsenic used in the present invention mainly uses what is obtained when caustic solution processing arsenic-containing smoke dust to contain
The solution of arsenic and tellurium.Arsenic content is high in solution, while 95% or more tellurium is enriched in solution, and recycles tellurium from high arsenic solution
The research of recycling arsenic has no relevant report.；
2, after the tellurium in flue dust is effectively dissolved and leached, the present invention selects the preferentially Selective Separation from leachate
Go out tellurium, lead, this is the characteristic based on arsenic, tellurium, lead, tin element in leachate so that tellurium, lead, tin selective reduction are from solution
Removing, the content of Te is up to 55% or more in purification slag；
3, labor intensity of the invention is low, processing time is short, good operational environment；
4, preparation process non-secondary pollution object generates, and can be enriched in arsenic after reduction in liquid, and arsenic is as zinc sulfate
Solution purification removes the raw material of cobalt nickel, is also of great significance in terms of environmental protection；
5, the removal efficiency of tellurium of the present invention has not only handled the alkali immersion liquid of tellurium containing arsenic, but also obtained pure 99% or more
NaAsO2, especially the rate of recovery of tellurium is up to 92% or more.
6, the rational process of the present invention is arranged in pairs or groups, by strictly controlling the conditional parameter in each process so that tellurium, arsenic obtain
It recycles and efficiently uses, achieved the purpose that environmentally friendly, economic, energy saving, high resource utilization, realize the recycling of arsenic and harmless
Change, and entire technique substantially three-waste free discharge, all resources obtain maximal efficiency utilization, and products therefrom is convenient for subsequent
Processing and processing, so the present invention has the advantage of environmentally friendly, economic, energy saving, high resource utilization.
Description of the drawings
Fig. 1 is the flow chart that metallic tellurium is obtained from containing arsenic, tellurium, lead, tellurium solution.
Specific implementation mode
It is the embodiment of the present invention below.
Embodiment 1：
By taking alkali immersion liquid in experiment as an example, wherein a concentration of Pb 706.67ppm of essential element, Sn 29.02ppm, Te
134.56ppm, As 28.29g/L, are handled using following steps：
(1) it neutralizes：H is added into alkali immersion liquid under conditions of temperature is 40 DEG C, mixing speed is 200r/min2SO4By alkali
The pH of immersion liquid is adjusted to 5, and solid-liquor separation obtains neutralizer and neutralizes slag；Gained neutralizes slag and enters follow-up hydrogen reduction process；
(2) selective reduction：Neutralizer enters selective reduction process obtained by step (1), and SO is passed through into neutralizer2,
The condition of control be gas flow be 2L/min, temperature is 60 DEG C, duration of ventilation 2h.It is molten that sodium arsenite is obtained after reduction
Liquid and reducing slag；
After testing：The content of each element is in reducing solution：Pb 2.86ppm, Sn 0.79ppm, Te 1.08ppm, As
27.01g/L.The removal efficiency of Pb and Te, which is calculated, is respectively：Pb 99.59%, Te 99.20%.
(3) hydrogen reduction and vacuum distillation：The neutralization slag of reducing slag and step (1) that step (2) obtains enters hydrogen reduction work
Sequence and vacuum distillation process, restore reducing slag in 600 DEG C, obtain 99.9% Te and lead skim, and lead skim is former as refining lead
Material；Then 99.9% Te is having there are two being evaporated in vacuo in the vacuum distillation furnace of condensation segment and a distilling period, and one section condenses
Temperature is 300 DEG C, two sections of condensation temperatures are 320 DEG C, distilling period temperature is 510 DEG C, vacuum degree 2Pa, and distillation obtains
99.999% high purity tellurium.
Embodiment 2：
By taking alkali immersion liquid in experiment as an example, wherein a concentration of Pb 647.26ppm of essential element, Sn 68.59ppm, Te
238.45ppm, As 38.46g/L, are handled using following steps：
(1) it neutralizes：H is added into alkali immersion liquid under conditions of temperature is 80 DEG C, mixing speed is 150r/min2SO4By alkali
The pH of immersion liquid is adjusted to 4, and solid-liquor separation obtains neutralizer and neutralizes slag；Gained neutralizes slag and enters follow-up hydrogen reduction process；
(2) selective reduction：Neutralizer enters reduction process obtained by step (1), and SO is passed through into neutralizer2, control
Condition be gas flow be 3L/min, temperature is 90 DEG C, duration of ventilation 3h.Sodium arsenite solution is obtained after reduction and is gone back
Former slag；
After testing：The content of each element is in reducing solution：Pb 2.43ppm, Sn 0.98ppm, Te 1.45ppm, As
37.89g/L.The removal efficiency of Pb and Te, which is calculated, is respectively：Pb 99.62%, Te 99.39%.
(3) hydrogen reduction and vacuum distillation：Reducing slag and the neutralization slag of step (1) enter hydrogen reduction process obtained by step (3)
With vacuum distillation process, reducing slag is restored in 650 DEG C, obtains 99.8% Te and lead skim, lead skim is as refining leady raw materials；
Then 99.7% Te is evaporated in vacuo in the vacuum distillation furnace of condensation segment and a distilling period there are two having, one section of condensation temperature
For 295 DEG C, two sections of condensation temperatures be 330 DEG C, distilling period temperature is 530 DEG C, vacuum degree 5Pa, distillation obtain 99.999% with
On high purity tellurium.
Embodiment 3：
By taking alkali immersion liquid in experiment as an example, wherein a concentration of Pb 547.85ppm of essential element, Sn 67.43ppm, Te
164.27ppm, As 19.44g/L, are handled using following steps：
(1) it neutralizes：H is added into alkali immersion liquid under conditions of temperature is 40 DEG C, mixing speed is 100r/min2SO4By alkali
The pH of immersion liquid is adjusted to 5, and solid-liquor separation obtains neutralizer and neutralizes slag；Gained neutralizes slag and enters follow-up hydrogen reduction process；
(2) selective reduction：Neutralizer obtained by step (1) enters reduction process, neutralizes slag and enters hydrogen reduction process.In
With SO is passed through in liquid2, the condition of control be gas flow be 5L/min, temperature is 70 DEG C, duration of ventilation 0.5h.Reduction terminates
After obtain sodium arsenite solution and reducing slag；
After testing：The content of each element is in reducing solution：Pb 3.04ppm, Sn 1.34ppm, Te 1.12ppm, As
18.51g/L.The removal efficiency of Pb and Te, which is calculated, is respectively：Pb 99.45%, Te 99.32%.
(3) hydrogen reduction and vacuum distillation：Reducing slag and the neutralization slag of step (1) enter hydrogen reduction process obtained by step (3)
With vacuum distillation process, reducing slag is restored in 620 DEG C, obtains 99.5% Te and lead skim, lead skim is as refining leady raw materials；
Then 99% Te is having there are two being evaporated in vacuo in the vacuum distillation furnace of condensation segment and a distilling period, and one section of condensation temperature is
310 DEG C, two sections of condensation temperatures be 315 DEG C, distilling period temperature is 500 DEG C, vacuum degree 3Pa, distillation obtain 99.99% or more
High purity tellurium.
Although above having used general explanation, specific implementation mode and experiment, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (7)
1. a kind of method for obtaining high purity tellurium in immersion liquid from alkali containing arsenic, which is characterized in that include the following steps：
(1) it neutralizes：The immersion liquid of alkali containing arsenic, the main component of the immersion liquid of alkali containing arsenic is taken to be：As 1~60g/L, Pb 50ppm~
800ppm, Sn 2ppm~200ppm, Te 10~120g/L of 10~500ppm, NaOH adjust the pH value of the immersion liquid of alkali containing arsenic
For 4-6, after solid-liquor separation, obtains neutralizer and neutralize slag, wherein neutralize slag and enter follow-up hydrogen reduction process；
(2) selective reduction：Reducibility gas is passed through into neutralizer obtained by step (1) to be restored, after reduction, liquid is solid
Reducing solution and reducing slag are obtained after separation；The reducing solution is pure sodium arsenite solution, is removed as the purification of solution of zinc sulfate arsenic
The raw material of cobalt nickel；
(3) hydrogen reduction, vacuum distillation：Reducing slag obtained by step (2) carries out hydrogen reduction with neutralization slag obtained by step (1), obtains thick
Tellurium and lead skim, lead skim is as refining leady raw materials, thick tellurium vacuum in the vacuum distillation furnace of condensation segment and a distilling period there are two having
Distillation, obtains 99.999% or more high purity tellurium.
2. according to the method described in claim 1, it is characterized in that：When being neutralized described in step (1) extremely controlled at room temperature
80℃。
3. method according to claim 1 or 2, it is characterised in that：Reducibility gas described in step (2) is SO2。
4. according to the method described in claim 3, it is characterized in that：In step (2), under the conditions of room temperature is to 90 DEG C, according to 0.5
The speed of~5L/min leads to SO2Gas time is 0.5~4h.
5. according to the method described in claim 1, it is characterized in that：In step (3), the temperature of the hydrogen reduction is 550 DEG C~
650℃。
6. method according to claim 1 or 5, it is characterised in that：In step (3), two condensation segments of vacuum distillation
Temperature is respectively 290 DEG C~310 DEG C and 310 DEG C~330 DEG C, and the temperature of distilling period is 500 DEG C~550 DEG C.
7. according to the method described in claim 6, it is characterized in that：The vacuum degree of vacuum distillation is 0.1~5Pa.
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| CN110894065B (en) * | 2019-12-18 | 2023-04-07 | 中南大学 | Equipment and method for preparing high-purity tellurium |
| CN111575491B (en) * | 2020-06-29 | 2021-11-19 | 株洲冶炼集团股份有限公司 | Resource comprehensive utilization method for purifying cobalt-nickel slag by zinc hydrometallurgy arsenic salt |
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| CN101844750A (en) * | 2010-06-04 | 2010-09-29 | 中南大学 | Method for preparing high-purity tellurium by material containing tellurium |
| CN102153054A (en) * | 2011-05-03 | 2011-08-17 | 嘉兴市达泽光电技术有限公司 | Preparation method of high purity tellurium |
| CN102874772A (en) * | 2012-09-17 | 2013-01-16 | 辽宁大学 | Method for preparing high-purity tellurium by using tellurium dioxide |
| CN102925703B (en) * | 2012-11-22 | 2014-04-30 | 湖南稀土金属材料研究院 | Method for recycling valuable metals from lead anode slime |
| CN104591104B (en) * | 2015-02-15 | 2016-08-24 | 江西铜业股份有限公司 | A kind of method reclaiming tellurium from low concentration is containing tellurium liquid |
| CN104911358B (en) * | 2015-06-10 | 2017-07-14 | 中南大学 | A kind of method that arsenic and selenium are separated in the alkaline leaching liquid from copper anode mud |
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