CN109485023A - A method of recycling tellurium from cupric tellurium waste liquid - Google Patents
A method of recycling tellurium from cupric tellurium waste liquid Download PDFInfo
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- CN109485023A CN109485023A CN201811550301.6A CN201811550301A CN109485023A CN 109485023 A CN109485023 A CN 109485023A CN 201811550301 A CN201811550301 A CN 201811550301A CN 109485023 A CN109485023 A CN 109485023A
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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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
- C25C5/02—Electrolytic production, recovery or refining of metal powders or porous metal masses from solutions
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Abstract
The method that the present invention provides a kind of to recycle tellurium from cupric tellurium waste liquid, comprising the following steps: S1, cupric tellurium waste liquid is subjected to electrodeposition at higher current densities, respectively obtains copper powder and the liquid of decopper(ing) containing tellurium；The cupric tellurium waste liquid is acidity, and wherein the concentration of copper is 10~70g/L；The high current density is in 400A/m2More than；The displacement that S2, the copper powder obtained using step S1 electrodeposition carry out tellurium to the liquid of decopper(ing) containing tellurium is enriched with, and is separated by solid-liquid separation, the tellurium copper slag being enriched with.The rate of recovery of tellurium of the present invention is up to 99.5%, and tellurium content is 45% or more in the tellurium copper slag of enrichment.Whole flow process of the present invention is coherent, brief; the below traditional handicraft such as equipment investment, occupied area, operating cost, environment influence, and can work continuously, continuous output high-quality tellurium copper slag; great amount of cost and operation are saved for subsequent purification technique, is suitable for industrial scale and promotes.
Description
Technical field
The invention belongs to small metal recovery refining techniques field more particularly to a kind of sides that tellurium is recycled from cupric tellurium waste liquid
Method.
Background technique
Tellurium metal content is rare, but uses extensively in certain specific areas, such as the cooling and warming of solar battery is just used
To tellurium；Tellurium is also used to the coloured material of the catalyst of cracking of oil, the brightener of electroplate liquid, glass；Tellurium can be added in steel
To increase its ductility, it is added to the intensity and corrosion resistance for increasing it in lead；Tellurium and its compound are a kind of semiconductor material again.
Currently, tellurium is mainly extracted from the waste liquid containing tellurium copper that copper anode mud is handled, after earth of positive pole high pressure leaches
Copper telluric acid liquid has become the main path of tellurium recycling.The more extracting method of industrial application are as follows: contained using the copper powder displacement of outsourcing
Tellurium in copper tellurium waste liquid, obtains telluride copper ashes.However, outsourcing copper powder generally has one layer of antioxidant covering, lead to displacement efficiency
It reducing, copper powder excess coefficient needs to reach 3 times or more in replacement process, and a large amount of copper powder excessively will cause the reduction of tellurium content,
The Purification of subsequent tellurium is difficult, and entire cost sharply increases.
Summary of the invention
In view of this, the application provides a kind of method for recycling tellurium from cupric tellurium waste liquid, method energy provided by the invention
Enough low costs expeditiously recycle the tellurium in acid solution, are suitable for industrial scale application.
The present invention provides a kind of method that tellurium is recycled from cupric tellurium waste liquid, comprising the following steps:
S1, cupric tellurium waste liquid is subjected to electrodeposition at higher current densities, respectively obtains copper powder and the liquid of decopper(ing) containing tellurium；It is described to contain
Copper tellurium waste liquid is acidity, and wherein the concentration of copper is 10~70g/L；The high current density is in 400A/m2More than；
The displacement that S2, the copper powder obtained using step S1 electrodeposition carry out tellurium to the liquid of decopper(ing) containing tellurium is enriched with, through solid-liquid point
From the tellurium copper slag being enriched with.
Preferably, the cupric tellurium waste liquid is sulfuric acid system, and wherein the concentration of copper is 20~55g/L.
Preferably, step S1 specifically: cupric tellurium waste liquid is added in Winning cell, recycles to be energised；In high current density
Lower electrodeposition is precipitated copper powder in cathode, while obtaining the liquid of decopper(ing) containing tellurium.
Preferably, the Winning cell has scraper plate, and the scraper plate periodically scrapes off the copper powder of precipitation.
Preferably, the anode of the Winning cell is lead anode, and cathode is stainless steel material；The circulation uses bottom in and top out
Mode, 1~2 cycle period per hour.
Preferably, the electrodeposition carries out at normal temperature, and current density is 400~1200A/m2。
Preferably, in step S2, the dosage for the copper powder that the electrodeposition obtains is within 3 times of displacement tellurium quality.
Preferably, for the reaction temperature of the displacement enrichment of the tellurium at 90 DEG C or more, the reaction time is 2.5~3h.
Compared with prior art, the embodiment of the present invention mainly carries out enriching and recovering to the tellurium in cupric telluric acid liquid, adopts first
Use 400A/m2Above current density, electrodeposition obtain copper powder, and a part of tellurium is precipitated and replaces during this, form decopper(ing) containing tellurium
Liquid；Then the present invention carries out the displacement of tellurium using electrodeposition copper powder, and recycling obtains tellurium copper slag.For the copper of 10~70g/L of copper concentration
Telluric acid liquid, when high current density electrodeposition of the present invention, anode generates a large amount of bubbles, reduces the concentration polarization of electric effusion,
Cathode crystal is precipitated fastly, and crystal grain is small, and generated bubble causes the copper powder of cathode to be enriched with conveying；High current density makes
Temperature increases, and high temperature is easy to overflowing for bubble and dissipates, more promotion copper electrodeposition.In replacement process of the present invention, because copper powder particle is thin
Small, active height, sufficiently, rapidly, tellurium content is high in final tellurium copper slag for reaction, to realize effective recycling enrichment of tellurium.Practice
Show the rate of recovery of tellurium of the present invention up to 99.5%, tellurium content is 45% or more in the tellurium copper slag of enrichment.
Whole flow process of the present invention is coherent, brief, and equipment investment, occupied area, operating cost, environment influence etc. below pass
System technique, and can work continuously, continuous output high-quality tellurium copper slag saves great amount of cost and operation for subsequent purification technique.
Detailed description of the invention
Fig. 1 is the process flow diagram of recycling tellurium provided in an embodiment of the present invention.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The method that the present invention provides a kind of to recycle tellurium from cupric tellurium waste liquid, comprising the following steps:
S1, cupric tellurium waste liquid is subjected to electrodeposition at higher current densities, respectively obtains copper powder and the liquid of decopper(ing) containing tellurium；It is described to contain
Copper tellurium waste liquid is acidity, and wherein the concentration of copper is 10~70g/L；The high current density is in 400A/m2More than；
The displacement that S2, the copper powder obtained using step S1 electrodeposition carry out tellurium to the liquid of decopper(ing) containing tellurium is enriched with, through solid-liquid point
From the tellurium copper slag being enriched with.
Referring to Fig. 1, Fig. 1 is the process flow diagram of recycling tellurium provided in an embodiment of the present invention.The embodiment of the present invention with
Acid cupric tellurium waste liquid is raw material, may be simply referred to as copper telluric acid liquid, for the acid solution containing copper, tellurium and some other impurity.
Wherein, the concentration of copper is 10~70g/L, preferably 20~55g/L；And the concentration of tellurium does not specially require.The cupric tellurium is useless
Liquid can be sulfuric acid system, such as the copper telluric acid liquid after the leaching of copper anode mud high pressure.In some embodiments of the invention, institute
Dense acid in the copper telluric acid liquid stated is 50~200g/L, and the present invention has no special limitation.
Cupric tellurium waste liquid is introduced into Winning cell by the embodiment of the present invention, is recycled to be energised；Electrodeposition at higher current densities,
Copper powder is precipitated in cathode, while obtaining the liquid of decopper(ing) containing tellurium.The electrodeposition of general copper be using insoluble anode, it is all heavy in electrolytic deposition process
Copper of the product on cathode all derives from copper solution, and copper concentration constantly declines in solution；Electrolysis and the cathode reaction of electrolytic deposition process are
The same.And the cupric tellurium waste liquid is added in the embodiment of the present invention in Winning cell, recycles to be energised.Specifically, the electrodeposition
The anode of slot is lead anode, and cathode is stainless steel material.Described to recycle the mode that bottom in and top out can be used, 1~2 is followed per hour
The ring period.
Also, the embodiment of the present invention carries out electrodeposition at higher current densities, and the high current density is in 400A/m2More than,
Preferably 400~1200A/m2, more preferably 500~1000A/m2, copper powder is in cathode precipitation.The electrodeposition is generally at normal temperature
It carries out, that is, is not necessarily to external heat source；The time of the electrodeposition can be 3h~6h.When high current density electrodeposition of the present invention, anode
A large amount of bubbles are generated, the concentration polarization of electric effusion is reduced, are precipitated fastly in cathode crystal, crystal grain is small, and generated
Bubble causes the copper powder of cathode to be enriched with conveying；High current density elevates the temperature, and high temperature is easy to overflowing for bubble and dissipates, more promotion copper
Electrodeposition.
In addition, the present invention uses high current density, the precipitation of a part of tellurium is also achieved during electrodeposition.The present invention
Some embodiments additionally use big cycle volume condition, such as circular flow is in 70L/h or more, this facilitate in liquid tellurium and precipitation
Copper powder occur a part displacement reaction, be achieved that the recycling of tellurium in electrolytic deposition process.
In a preferred embodiment of the invention, the Winning cell has scraper plate, and the scraper plate periodically scrapes the copper powder of precipitation
From.The embodiment of the present invention by copper powder periodically scrape off, it can be achieved that in liquid copper powder recycling, and in air insulated play protection make
With ensure that the quality of copper powder.Homemade Winning cell can be used in the embodiment of the present invention, for scraper plate and under taper
The trough of material mouth, but material is not particularly limited, the corrosion-resistant condition at scene can be met.
Electrodeposition of the embodiment of the present invention obtains copper powder, and a part of tellurium is precipitated and replaces during this, forms the liquid of decopper(ing) containing tellurium；It should
Decopper(ing) liquid is usually the slurry form containing tellurium, also referred to as liquid after electrodeposition.After electrodeposition operation, the embodiment of the present invention will contain tellurium decopper(ing)
Liquid is put into reactive tank, is enriched with, is then separated by solid-liquid separation, the tellurium copper being enriched with using the displacement that the copper powder that electrodeposition obtains carries out tellurium
Slag.In replacement process of the present invention because copper powder particle is tiny, active height, reaction sufficiently, rapidly, the tellurium copper slag recycled
Middle tellurium content is high.
It is more for outsourcing copper powder direct replacement tellurium in current tellurium recovery process, obtain cuprous telluride and copper powder, copper oxygen
The mixture of compound etc., ingredient is single, copper content is generally greater than 40%, tellurium is lower than 30%, and prior, actually copper powder
Additional amount is usually 4 times of theoretical amount or more, wherein the copper powder for having unreacted copper powder and being dissolved into copper liquid.Current commercially available copper
Powder is oxidizable in air because particle is thinner, so complicated anti-oxidant treatment and crystal grain refinement processing are all done in storage,
And copper powder price is higher than at least 0.5 ten thousand yuan/ton of 4N cathode copper processing, in addition because by processing, higher temperature, longer reaction
Time etc., technical process is cumbersome, and cost is very high.
The present invention uses high current density electro deposited copper powder substitution tellurium, and gained copper powder can be personal in the entire circulatory system, directly
It taps into the heavy tellurium of heavy tellurium slot, avoids and refine some pairs of unnecessary operations of this technique such as crystal grain, anti-oxidant, and because without
Processing, the surface-active of copper powder is more preferable, and the reaction temperature in heavy tellurium is lower, the time is shorter, has low cost, high efficiency etc. excellent
Gesture.
In an embodiment of the present invention, the dosage for the copper powder that the electrodeposition obtains is within 3 times of displacement tellurium quality, generally
It is 2~3 times.The embodiment of the present invention releases liquid after the copper powder and electrodeposition, is added in reaction kettle and heats, and preferably stirring is replaced
Reaction.The reaction temperature of the displacement enrichment of the tellurium is preferably at 90 DEG C or more, and more preferably 90~100 DEG C；Reaction time can be
2.5h~3h.
Material after displacement reaction is separated by solid-liquid separation by the embodiment of the present invention, and the separation of solid and liquid can be art technology
The modes such as filtering, suction filtration known to personnel, respectively obtain tellurium copper slag and waste liquid.The tellurium copper slag can carry out proposing tellurium processing；It is described
Waste liquid is known as displaced liquid, can outlet progress electrodeposition decopper(ing).In an embodiment of the present invention, obtained tellurium copper slag is mainly
The mixture of tellurium, the oxide of tellurium, cuprous telluride etc., to provide convenience in the purification processes of later tellurium copper slag.In the present invention
Electro deposited copper copper after copper tellurium liquid, electrodeposition reduces, and copper part returns to tail washings after replacing tellurium, makes subsequent tail washings processing cost more
It is low.
Practice have shown that the rate of recovery of tellurium of the present invention, up to 99.5%, tellurium content reaches in the tellurium copper slag of enrichment
45%.The present invention technique whole flow process is coherent, brief, it is easy to accomplish, and since the copper powder activity that electrodeposition goes out is strong, significantly
Subsequent time swap and technological operation difficulty are shortened, process equipment is simple, and industrialization occupied area is small, and it is at low cost, to ring
Border is friendly, and tellurium content is much higher than the tellurium content of traditional replacement method in obtained tellurium copper slag, is suitable for industrial scale and promotes.
For a further understanding of the application, tellurium is recycled from cupric tellurium waste liquid to provided by the present application below with reference to embodiment
Method be specifically described.
In following embodiment, elemental composition detection is carried out according to conventional method in that art；Reagent used is commercially available production
Product.
Embodiment 1
Winning cell is installed first, which is with scraper plate, the trough with taper feed opening, and Anodic is lead sun
Pole, cathode are stainless steel material.
Using the endless form of bottom in and top out, the Winning cell is added in 80L copper telluric acid liquid and is recycled, flow 80L/h.
It is powered at normal temperature, current density 550A/m2, electrodeposition time 6h, copper powder is in cathode precipitation, the regular (120S of Winning cell scraper plate
Scrape primary) copper powder is scraped off.Then, release electrodeposition after liquid and electrodeposition obtain copper powder (specially before electrodeposition in liquid tellurium content 3
Times), it is added in reaction kettle and is heated to 90 DEG C, be stirred to react 3h, filter, respectively obtain 1327g tellurium copper slag and waste liquid 71.5L.
Data see the table below, and can be seen that from 1 result of table, during electrodeposition copper powder, tellurium decline 14.7%, and replace after tellurium product
Position reaches 45% or more.
The data statistics of 1 embodiment 1 of table recycling tellurium
Embodiment 2
Winning cell (with embodiment 1) is installed, using the endless form of bottom in and top out, the electricity is added in 80L copper telluric acid liquid
Product slot is recycled, flow 70L/h.It is powered at normal temperature, current density 750A/m2, electrodeposition time 3.5h, copper powder is in yin
Pole is precipitated, and Winning cell scraper plate periodically (120S is scraped once) scrapes off copper powder.Then, the copper powder that liquid and electrodeposition obtain after releasing electrodeposition
(3 times of tellurium content in liquid specially before electrodeposition) is added in reaction kettle and is heated to 92 DEG C, be stirred to react 2.7h, filter, respectively
To 984g tellurium copper slag and waste liquid 73L.
Data see the table below, and can be seen that from 2 result of table, during electrodeposition copper powder, tellurium decline 40.82%, and tellurium after replacing
Grade reaches 45% or more.
The data statistics of 2 embodiment 2 of table recycling tellurium
Embodiment 3
Winning cell (with embodiment 1) is installed, using the endless form of bottom in and top out, the electricity is added in 80L copper telluric acid liquid
Product slot is recycled, flow 100L/h.It is powered at normal temperature, current density 950A/m2, electrodeposition time 4h, copper powder is in yin
Pole is precipitated, and Winning cell scraper plate periodically (120S is scraped once) scrapes off copper powder.Then, the copper powder that liquid and electrodeposition obtain after releasing electrodeposition
(3 times of tellurium content in liquid specially before electrodeposition) is added in reaction kettle and is heated to 96 DEG C, be stirred to react 2.5h, filter, respectively
To 1250g tellurium copper slag and waste liquid 67L.
Data see the table below, and can be seen that from 3 result of table, during electrodeposition copper powder, tellurium decline 21.16%, and tellurium after replacing
Grade reaches 45% or more.
The data statistics of 3 embodiment 3 of table recycling tellurium
As seen from the above embodiment, the present invention uses high current density electro deposited copper telluric acid liquid for the first time, one in electrolytic deposition process
Divide tellurium to be precipitated and be replaced, recycle the remaining tellurium of copper powder displacement decopper(ing) liquid of electrodeposition, the rate of recovery of tellurium is enriched with up to 99.5%
Tellurium copper slag in tellurium content 45% or more.The present invention realizes effective recycling enrichment of tellurium；Whole flow process of the present invention is coherent, simple
It is short, the below traditional handicraft such as equipment investment, occupied area, operating cost, environment influence, and can work continuously, it is continuous to produce
High-quality tellurium copper slag out saves great amount of cost and operation for subsequent purification technique.
The above is only a preferred embodiment of the present invention, it is noted that for making the professional technique of the art
Personnel are that by various modifications to these embodiments without departing from the technical principles of the invention, and these
Modification also should be regarded as the range that the present invention should protect.
Claims (8)
1. a kind of method for recycling tellurium from cupric tellurium waste liquid, comprising the following steps:
S1, cupric tellurium waste liquid is subjected to electrodeposition at higher current densities, respectively obtains copper powder and the liquid of decopper(ing) containing tellurium；The cupric tellurium
Waste liquid is acidity, and wherein the concentration of copper is 10~70g/L；The high current density is in 400A/m2More than；
The displacement that S2, the copper powder obtained using step S1 electrodeposition carry out tellurium to the liquid of decopper(ing) containing tellurium is enriched with, and is separated by solid-liquid separation, is obtained
To the tellurium copper slag of enrichment.
2. wherein copper is dense the method according to claim 1, wherein the cupric tellurium waste liquid is sulfuric acid system
Degree is 20~55g/L.
3. the method according to claim 1, wherein step S1 specifically: it is useless that cupric tellurium is added in Winning cell
Liquid recycles to be energised；Electrodeposition at higher current densities is precipitated copper powder in cathode, while obtaining the liquid of decopper(ing) containing tellurium.
4. according to the method described in claim 3, the scraper plate periodically will be negative it is characterized in that, the Winning cell has scraper plate
The copper powder that pole is precipitated scrapes off.
5. according to the method described in claim 3, cathode is stainless it is characterized in that, the anode of the Winning cell is lead anode
Steel material；The circulation is by the way of bottom in and top out, 1~2 cycle period per hour.
6. method according to any one of claims 1 to 5, which is characterized in that the electrodeposition carries out at normal temperature, electric current
Density is 400~1200A/m2。
7. according to the method described in claim 6, it is characterized in that, in step S2, the dosage for the copper powder that the electrodeposition obtains is
Within 3 times for replacing tellurium quality.
8. the method according to the description of claim 7 is characterized in that the tellurium displacement enrichment reaction temperature 90 DEG C with
On, the reaction time is 2.5~3h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811550301.6A CN109485023B (en) | 2018-12-18 | 2018-12-18 | Method for recovering tellurium from copper-tellurium-containing waste liquid |
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| CN201811550301.6A CN109485023B (en) | 2018-12-18 | 2018-12-18 | Method for recovering tellurium from copper-tellurium-containing waste liquid |
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| CN111378990A (en) * | 2020-04-27 | 2020-07-07 | 阳谷祥光铜业有限公司 | Electrodeposition impurity removal process for 6N copper electrolyte |
| CN112174099A (en) * | 2020-09-17 | 2021-01-05 | 中南大学 | Method for separating tellurium from copper-tellurium-containing complex acidic solution |
| CN112499598A (en) * | 2020-11-12 | 2021-03-16 | 阳谷祥光铜业有限公司 | Method for extracting tellurium from copper anode slime press leaching solution |
| CN113564622A (en) * | 2021-08-09 | 2021-10-29 | 安徽工业大学 | Method for efficiently separating copper and tellurium from copper telluride material |
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| CN113564622A (en) * | 2021-08-09 | 2021-10-29 | 安徽工业大学 | Method for efficiently separating copper and tellurium from copper telluride material |
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|---|---|
| CN109485023B (en) | 2021-10-22 |
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