CN104928483B - Method for comprehensively recovering silver, selenium, tellurium and copper from copper telluride residues - Google Patents
Method for comprehensively recovering silver, selenium, tellurium and copper from copper telluride residues Download PDFInfo
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Abstract
The invention discloses a method for comprehensively recovering silver, selenium, tellurium and copper from copper telluride residues. The method comprises the following steps: (1) oxidation acid leaching: adding copper telluride slag into a dilute sulfuric acid solution containing an oxidant, heating, stirring, leaching, filtering to obtain a copper sulfate leaching solution and an acid leaching slag, and recycling copper from the leaching solution; (2) alkaline leaching and separating: adding the acid leaching residue into a sodium hydroxide solution for leaching to obtain a sodium tellurite solution and an alkaline leaching residue, and returning the alkaline leaching residue to a KALDO furnace for smelting to recover silver and selenium; and purifying the alkali leaching solution, precipitating tellurium, calcining and electrolyzing to prepare refined tellurium. The method provided by the invention has the advantages of high recovery rate of silver, selenium, tellurium and copper, no loss of silver, selenium, tellurium and copper, high enrichment ratio, good separation from other impurities, small environmental pollution, simple process and low cost of required equipment.
Description
Technical field
The invention belongs to hydrometallurgy field of engineering technology, and in particular to a kind of telluride copper ashes Comprehensive Recovery of Ag, selenium, tellurium,
The method of copper.
Background technology
Contain a certain amount of tellurium in copper anode mud.In KALDO stove handling process, copper anode mud adds the pre- immersion trough of normal pressure,
Liquid and process water after sulfuric acid, heavy tellurium are mended, logical to be steam heated to 80 DEG C, drum air or oxygen leaching makes part copper by solid phase
Liquid phase is transferred to, supernatant entered rate and sends into net liquid workshop processing recovery copper；The slurry feeding autoclave precipitated, leads to steam liter
Temperature leads to oxygen leaching, impurity is transferred to liquid phase by slag phase, reaction terminates, and slurry is transferred in acid condition to 120 DEG C
Pressure leaching transhipment groove cooling, then filter press progress separation of solid and liquid is pumped, filter cake is wet decopper(ing) mud, spiral feeding double helix steam drying
Machine, is dried to aqueous 1%-3%；The silver-colored selenium groove of filtrate feeding leads to sulfur dioxide, makes silver-colored selenium precipitate reduction, enters being pumped into filter press
Row separation of solid and liquid, filter cake is that silver-colored selenium slag enters Kaldo Furnace recovery, and filtrate enters heavy tellurium groove, plus copper powder, leads to steam heating, reduces tellurium
Precipitation, carries out separation of solid and liquid, filter cake is telluride copper ashes in pumping filter press.
Tellurium is carried in the telluride copper ashes obtained from displacement mainly oxidation acid leaching and alkali oxide leaching both approaches, also has neutrality
The leaching methods such as Oxidation Leaching, acidic oxidation complexation leaching, but the only single recovery for considering tellurium of these methods, and to telluride copper
The synthetical recovery of the valuable metal such as the higher silver of content, selenium, copper considers less in slag.The tellurium of certain Tong Ye company synthesis workshop output
Change copper ashes drying sample, its chemical composition is：Copper 18.07%, silver 30.06%, tellurium 19.56%, selenium 7.58%；Other 24.71%,
Therefore, design telluride copper ashes synthetical recovery tellurium process program when, consider copper, tellurium, silver, the enrichment of four kinds of elements of selenium and
Separation with other impurities is very necessary.
The content of the invention
Present invention aim to provide a kind of method of telluride copper ashes Comprehensive Recovery of Ag, selenium, tellurium, copper.
The present invention is achieved through the following technical solutions：
A kind of telluride copper ashes Comprehensive Recovery of Ag, selenium, tellurium, the method for copper, this method are carried out as steps described below：
(1) oxidation acid leaching：Liquid-solid ratio 3 is pressed in acid-resistant container:1 adds water and tellurium copper slag, sequentially adds under agitation dense
Sulfuric acid and copper sulphate, the wherein concentrated sulfuric acid and copper sulphate account for the 30-40% and 1-6% of tellurium copper slag weight respectively；Then it is continually fed into
Air is simultaneously stirred, and is heated to after 90 DEG C, and the combined oxidation agent solution being made up of sodium chlorate and sodium chloride is instilled in 2h, wherein
Sodium chlorate and sodium chloride account for the 10-13% and 4-7% of tellurium copper slag weight respectively, react 1-1.5h after dripping off again；Filter, filter while hot
Slag hot wash 3 times, it is copper-bath to merge diafiltration liquid；Filter residue is the acid leaching residue of the silver-colored selenium containing tellurium；
(2) alkali leaching separation：Liquid-solid ratio 5-6 is pressed in reaction vessel:It is wet after whole washing filterings that 1 above-mentioned reaction is obtained
Acid leaching residue and water, are then added portionwise sodium hydrate solid and industrial sodium sulfide, wherein NaOH and sulphur by several times under agitation
Change 38-45% and 10-15% that sodium accounts for tellurium copper slag weight respectively, more than 60-80 DEG C, stirring reaction are heated to after adding
1h；Filter while hot, filter residue hot wash, it is the alkali leaching solution for obtaining sodium tellurite to merge diafiltration liquid, alkali immersion liquid is purified, heavy
Smart tellurium is made after tellurium, calcining, electrolysis；Alkali leaching slag is to be enriched silver, the silver-colored selenium slag of selenium, and alkali phase analysis is sent the melting of KALDO stoves back to and returned
Cash register, selenium.
Compared with prior art, the beneficial effects of the present invention are：
The know-why of the present invention is as follows：
(1) oxidation acid leaching mechanism：
Cu2Te is in the presence of an oxidizer, it is easy to forms tellurous acid or tellurite with acid and alkali reaction, and is transferred to it
Solution：
Cu2Te+2H2SO4+2O2====H2TeO3+2CuSO4+H2O
Cu2Te+2NaOH+3/2O2====Na2Te03+Cu2O+H2O
The Na for being difficult to be dissolved by alkali lye can be formed if over oxidation2Te04Compound.The leaching of over oxidation alkali then may be by tellurium
It is oxidized to the Cu of more indissoluble3Te06(this telluric acid copper is in emerald green).
In addition, containing substantial amounts of copper, silver and selenium in tellurium copper slag, wherein silver element is needed to the leaching of tellurium by large effect
Silver is changed into silver nitride precipitation while decopper(ing).
(2) alkali leaching separating mechanism
Tellurium copper slag is after oxidation acid leaching, and the tellurium in leached mud is main with TeO2、CuTeO3Etc. form exist, and silver then with
AgCl、Ag2The forms such as O are present, and selenium is with Se, SeO2、SeO3、CuSeO3Exist etc. form.The chemical property of tellurium and sulphur and selenium phase
Closely, but tellurium compared with sulphur and selenium with more alkalescence, tellurium dioxide is soluble in strong base solution and generates tellurite (such as Na2TeO3Deng).Alkali
Leaching method optionally dissolution can dissolve in the material of alkaline solution, tellurium is dissolved in alkaline solution and is resided in most metals
In slag.Chemical equation is：
TeO2+ NaOH====Na2TeO3+H2O
Na2S+CuTeO3====CuS ↓+Na2TeO3
(3) wet cleaning mechanism
Containing impurity such as a small amount of Se, Cu, Pb, Si in alkali leaching solution, the electrodeposition of next step tellurium is influenceed, it is necessary to by refined
The most of impurity of removing.This experiment added in the sodium tellurite solution that alkali soaks appropriate vulcanized sodium, calcium chloride can remove it is insoluble
In impurity such as the impurity and Cu, Pb, Si of alkali lye.Chemical equation is as follows：
TeO2+ NaOH====Na2TeO3+H2O
Na2S+Na2PbO2+2H2O====PbS ↓+4NaOH
Na2S+Na2CuO2+2H2O====CuS ↓+4NaOH
Sodium tellurite solution after purification and impurity removal, it is 3-5 that pH value is neutralized to dilute sulfuric acid, is precipitated as obtaining after scrubbed drying
To refined TeO2Product, the TeO2Sediment is the base stock of electrowinning tellurium.Chemical equation is as follows：
CaCl2+2Na2SiO3====CaSiO3↓+2NaCl
Na2TeO3+H2SO4====TeO2↓+Na2SO4+H2O
It is pointed out that the TeO2 products after wet separation is refined are higher containing selenium, and selenium works as tellurium in tellurium electrolytic deposition process
When concentration is relatively low, current density is higher, electrodeposition tellurium grade will be influenceed.Therefore should be de- using calcining volatilization containing the high TeO2 products of selenium
Selenium.400 DEG C of temperature is controlled, bed of material thickness 10mm calcines 4h, Se content can be reduced into 0.001%-0.005%.
(4) tellurium electrodeposition founding mechanism
With TeO2It is electrolysed for raw material electrodeposition method from the sodium hydroxide solution of sodium tellurite, it is 99% that can deposit purity
Metallic tellurium above, electrodeposition tellurium product is after founding removal of impurities, and quality disclosure satisfy that non-ferrous metal industry standard YS/T222-2010
《Tellurium ingot》It is required that.The tellurium electrodeposition principles of chemistry are：
Total electrodeposition reaction：Na2TeO3+H2O===Te ↓+2NaOH+O2↑
Anode：4OH-===2H2O+O2↑+4e E-=-0.57V
Negative electrode：TeO3 2-+3H2O+4e===Te ↓+6OH-E-=0.40V
Precipitations of major control impurity Pb, the Se on negative electrode tellurium in electrolysis, when tellurium concentration is relatively low, current density is higher,
Because Pb, Se deposition potential and Te are sufficiently close to, Pb and Se precipitation are more notable：
PbO2 2-+2H2O+2e====Pb+4OH-E-=-0.54V
SeO3 2-+3H2O+4e====Se+6OH-E-=-0.366V
It can be seen that Pb, Se deep removal are very important to the grade for ensureing electrodeposition tellurium in advance before tellurium electrodeposition.In addition,
Because Te is constantly while negative electrode is separated out, the NaOH of respective amount will be also generated simultaneously, can be in electrode when NaOH concentration is too high
The local supersaturation in surface is separated out, and electrodes conduct is deteriorated electrode surface covering, and tank voltage rise causes impurity to separate out increase,
Therefore the Te concentration that electrodeposition is ended can not be too low.
NaOH viscosity is big in electrolyte during due to electrodeposition tellurium, and NaOH can cause product containing sodium in micro entrance metallic tellurium
It is unqualified, therefore, must in casting product tellurium, control casting temperature for 550-650 DEG C, agitation melt, utilize tellurium and NaOH
Fusing point (450 DEG C and 318 DEG C) and density (6.24g/cm3With 2.13g/cm3) difference, sodium is floated into slag and remove.If electrodeposition
It is preceding by Pb, Se deep removal, the electrodeposition tellurium grade that an electrodeposition is obtained can reach 99.998%.
Brief description of the drawings
Fig. 1 is telluride copper ashes Comprehensive Recovery of Ag, selenium, tellurium, process for copper flow chart.
Embodiment
The present invention is described further below：
Embodiment one：Telluride copper ashes oxidation acid leaching decopper(ing) is tested
Experiment telluride copper ashes used is the tellurium of the comprehensive workshop output of Tong Ye companies of Baiyin Nonferrous Metal Group Co., Ltd.
Change copper ashes wet feed, its water content is 36-38%, in 2000ml beakers, the wet tellurium copper slag 500g of addition (based on drying amount 64%,
Solid is 320g), (liquid-solid ratio is 3 to the 800ml that adds water:1) slurry, is stirred into；Then 93% industrial sulphur is sequentially added under agitation
Sour 40ml, cupric sulfate pentahydrate 32g；Be heated to more than 90 DEG C, be continually fed into air in reaction ore pulp and stir, instilled in 2h by
Oxidant 55g, salt 25g, the composite oxidant SC solution of water 250g dissolvings, react 1-1.5h again after dripping off；Filter while hot,
Filter residue hot wash 3 times, it is that copper-bath is 1700ml to merge diafiltration liquid；Filter residue is that the acid leaching residue of the silver-colored selenium containing tellurium is wet
Measure as 466.46g, its contents on dry basis is 65.8%.
Experimental result is as shown in table 1.
The oxidation acid leaching experimental result of table 1
In 2000ml beakers, the wet acid leaching residue added after whole filtering washings that above-mentioned reaction is obtained, add water 1500ml
(liquid-solid ratio is 5-6:1)；Then sodium hydrate solid 150g and industrial sodium sulfide 58g is added portionwise by several times under agitation, adds
After be heated to more than 60-80 DEG C, stirring reaction 1h；Filter while hot, filter residue hot wash three times, merge diafiltration liquid and produce
To the alkali leaching solution about 2560ml of sodium tellurite；Alkali leaching slag is to be enriched silver, the silver-colored selenium slag of selenium, is after slag drying
174.14g。
Alkali leaching experimental result is as shown in table 2.As shown in Table 2, can be by when carrying out immersion liquid leaching to slag after acidleach
92.49% tellurium is changed into sodium tellurite and leached into alkali lye, but is soluble in the solution containing a small amount of copper, selenium, lead, silicon etc.
The impurity component of alkali lye is, it is necessary to which further impurity and purification could be used for electrodeposition tellurium.100% silver is enriched in tailings after alkali leaching
With 94.21% selenium, wherein copper, tellurium, silver, the content of selenium respectively reach 12.11%, 2.68%, 56.75%, 12.87%, can
Return to KALDO stoves smelting system or carry out secondary oxidation acidleach and copper, tellurium, silver, selenium is separately recovered.
The alkali of table 2 extracts tellurium experimental result
Embodiment three：Wet cleaning prepares TeO2Product is tested
The whole alkali leaching solution of 2560ml that above-mentioned reaction is obtained are put into 3000ml beakers, under stirring at normal temperature, successively
EDTA solution 0.1g, anhydrous calcium chloride powder 5g, vulcanized sodium powder 5g are added, continues stirring reaction 2h, stands overnight, it is sunk
Starch is grown up and fully settled.Next day filters the solution after whole removal of impurities, obtains light yellow transparent solution 2570ml.Cross filter residue
For removal of impurities slag, 17.3g is dried to obtain, the high pressure that can return to KALDO stoves leaches process secondary recovery copper, tellurium.
The whole clarified solutions obtained after removal filtration are fitted into 3000ml beakers, agitating device is installed, is heated to 60
More than DEG C, the 1+3 dilute sulfuric acids prepared in advance are slowly added under agitation (1 part of 98% reagent grade sulfuric acid and 3 parts of water are mixed)
Neutralized, until solution ph is 3.0-4.5,1+3 sulfuric acid 460mL consumed altogether, go out sediment with isolated by vacuum filtration while hot,
Then with a small amount of hot water filter wash repeatedly, discharge neutralizes waste water 3010mL altogether；By the TeO being filtrated to get2Sediment wet feed all dries
Dry, weight obtains 76.60g.
Impurity and purification prepare TeO2The experimental result of product is as shown in table 3.To refining TeO2Product sample presentation makees full elemental analysis
As a result it is as shown in table 4.
The impurity and purification experimental result of table 3 and account
Table 4 refines TeO2Product full elemental analysis result (total amount 93.8%)
| Element | Te | Cu | Se | O | Na |
| Content % | 64.62 | 0.03475 | 2.525 | 22.40 | 1.546 |
| Element | S | As | Zn | Si | Mg |
| Content % | 0.3896 | 0.1291 | 0.00975 | 0.3057 | 0.1546 |
| Element | Al | Ca | Fe | Pb | Cl |
| Content % | 0.1729 | 0.09517 | 0.0963 | 0.05927 | 0.3458 |
From the result of table 3, table 4, after alkali leaching liquor wet cleaning removal of impurities, in removal of impurities slag it is main be enriched copper, tellurium,
The elements such as lead, sulphur, wherein cupric 7.03%, containing tellurium 9.31%, the high pressure that the slag can return to KALDO stoves leaches process secondary recovery
Copper, tellurium.Wet cleaning can deviate from the metal impurities such as copper in solution, lead, and extrusion rate is up to more than 96.9%, but wet cleaning can not
The selenium deviate from selenium, aqueous slkali exists in sodium selenite form, and SeO is formed when acid is neutralized2Precipitation is all enriched to TeO2Product
In.The TeO that scavenging solution neutralization precipitation is obtained2Tellurium grade is up to 71.87% in product, and the tellurium rate of recovery is up to 95.83%, and selenium grade is
2.84%, selenium recovery is 100%, the TeO2Product can as electrodeposition tellurium raw material.
Example IV：Tellurium electrodeposition is tested
The experiment of tellurium electrodeposition is carried out in laboratory, experiment TeO used2Product is the pilot scale TeO that tellurium slag project pilot scale is obtained2
Product, its grade containing tellurium is 69.49%, and electrodeposition experiment twice shares wet TeO2Product 15kg(solid content 22-23%).Experiment institute
It is that poly (methyl methacrylate) plate is made by oneself with electrolytic cell, Winning cell volume=long 28cm × wide 12cm × depth 15cm=5.0L, actual load electrolyte
4-4.5L.Electrodeposition is made of positive plate using iron plate, and minus plate is made using stainless steel, and monolithic minus plate electrodeposition area=
0.096m×0.100m×2≈0.02m2；Power supply is electrolysed electroplating power supply equipment by SDD-1250 and provided.
With 8L rustless steel containers as reaction unit, the residual solution 4.0L added after first time electrodeposition, benefit adds water to total
Volume is 5.0L or so, then adds refined TeO of the powdery containing tellurium 69.49%2Product 1100g, adds solid sodium hydroxide
500g, stirring 2h is allowed to abundant dissolving.The solution left standstill storage 24h prepared, then uses siphon by supernatant liquid (about 4.0L)
Method is extracted out and pours into electrolytic cell.The electric effusion concentration containing tellurium is analyzed for 164.21g/L through sample presentation.
Insertion takes 2 pieces of minus plates in a cell, and 3 pieces of positive plates switch on power, and its electric current is adjusted with universal meter is
4.8A, voltage is 3.8V, is stopped after continuous electrodeposition 42h, now electrodeposition tellurium is attached on minus plate in the form of sheets.By two after electrodeposition
Block minus plate is extracted out, is washed with 5% oxalic acid solution, then is washed till neutrality with clear water, is then dried, is weighed as 250.9g, the negative electrode
Tellurium sample presentation analysis grade containing tellurium is 99.5%.Residual solution after tellurium electrodeposition is poured out from electrolytic cell, volume about 4000ml clarifications, bottom
Only a small amount of sediment, it is 101.8g/L that sample presentation, which analyzes it containing tellurium,.Liquid is higher containing tellurium after the electrodeposition, can add TeO2Liquid making again,
Return to next round electrodeposition.
To sum up embodiment, which is calculated, is understood, after a leaching operation, the rate of recovery of four kinds of valuable metals is respectively reached：Copper
69.4-85.76%, tellurium 88.95-95%, silver 94.9%, selenium 90.35%.The leaching slag charge of generation returns to KALDO stove main flows
After being recycled through secondary cycle, copper, tellurium, silver, the comprehensive recovery of four kinds of valuable metals of selenium all can reach more than 95%.
Claims (1)
1. a kind of telluride copper ashes Comprehensive Recovery of Ag, selenium, tellurium, the method for copper, it is characterised in that：Described method is as steps described below
Carry out：
（1）Oxidation acid leaching：Liquid-solid ratio 3 is pressed in acid-resistant container:1 adds water and tellurium copper slag, the hundred of each element wherein in tellurium copper slag
Point content ratio is:Cu is that 18.075, Te is that 19.565, Ag is 30.065 and Se is 7.585, and dense sulphur is sequentially added under agitation
Acid and copper sulphate, the wherein concentrated sulfuric acid and copper sulphate account for the 30-40% and 1-6% of tellurium copper slag weight respectively；Then it is continually fed into air
And stir, it is heated to after 90 DEG C, the combined oxidation agent solution being made up of sodium chlorate and sodium chloride, wherein chloric acid is instilled in 2h
Sodium and sodium chloride account for the 10-13% and 4-7% of tellurium copper slag weight respectively, react 1-1.5h after dripping off again；Filter while hot, filter residue heat
Water washing 3 times, it is copper-bath to merge diafiltration liquid；Filter residue is the acid leaching residue of the silver-colored selenium containing tellurium；
（2）Alkali leaching separation：Liquid-solid ratio 5-6 is pressed in reaction vessel:It is wet after whole washing filterings that the 1 above-mentioned reaction of addition is obtained
Acid leaching residue and water, are then added portionwise sodium hydrate solid and industrial sodium sulfide, wherein NaOH and sulphur by several times under agitation
Change 38-45% and 10-15% that sodium accounts for tellurium copper slag weight respectively, 60-80 DEG C, stirring reaction 1h are heated to after adding；While hot
Filtering, filter residue hot wash, it is the alkali leaching solution for obtaining sodium tellurite to merge diafiltration liquid, and alkali immersion liquid is purified, heavy tellurium, forge
Smart tellurium is made after burning, electrolysis；Alkali leaching slag be enriched silver, the silver-colored selenium slag of selenium, alkali phase analysis send back to the melting of KALDO stoves reclaim silver,
Selenium.
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| CN105347315A (en) * | 2015-11-18 | 2016-02-24 | 金川集团股份有限公司 | Method for extracting crude tellurium from tellurium-containing smelting waste residue |
| CN106381399B (en) * | 2016-09-27 | 2018-10-02 | 郴州市金贵银业股份有限公司 | A method of recycling tellurium from high tellurium slag charge |
| CN106757118B (en) * | 2016-12-08 | 2019-03-01 | 湖南稀土金属材料研究院 | The method of smart tellurium is extracted from antimony tellurium waste material |
| CN107142377B (en) * | 2017-04-27 | 2018-12-21 | 永兴鑫裕环保镍业有限公司 | The technique of extracting and developing copper and tellurium from copper tellurium slag |
| CN109112560A (en) * | 2018-09-19 | 2019-01-01 | 云南铜业股份有限公司西南铜业分公司 | A method of high purity tellurium is prepared using copper telluride |
| CN109207733B (en) * | 2018-09-26 | 2020-06-30 | 云南铜业科技发展股份有限公司 | Preparation method for extracting tellurium from tellurium copper slag |
| CN109371238A (en) * | 2018-10-30 | 2019-02-22 | 金川集团股份有限公司 | A method of removing selenium from noble metal concentrate |
| CN111204716A (en) * | 2020-03-06 | 2020-05-29 | 大冶有色金属有限责任公司 | Process method for refining crude tellurium |
| CN111498815A (en) * | 2020-04-28 | 2020-08-07 | 吉林大学 | High-pressure preparation method of orthorhombic phase copper-tellurium oxide |
| CN112593245A (en) * | 2020-12-09 | 2021-04-02 | 广东先导稀贵金属材料有限公司 | Purification and recovery process of crude tellurium |
| CN112695199A (en) * | 2020-12-15 | 2021-04-23 | 广东先导稀贵金属材料有限公司 | Method for extracting tellurium and copper from tellurium-copper slag |
| CN112520707A (en) * | 2020-12-28 | 2021-03-19 | 广东先导稀贵金属材料有限公司 | Preparation method of tellurium dioxide |
| CN114959278B (en) * | 2022-04-25 | 2024-02-20 | 金川集团股份有限公司 | Method for efficiently separating and recovering copper and tellurium from copper-tellurium slag |
| CN115215303A (en) * | 2022-06-22 | 2022-10-21 | 白银有色集团股份有限公司 | Method for extracting tellurium dioxide from tellurium copper slag |
| CN115432672B (en) * | 2022-07-20 | 2023-12-29 | 西北矿冶研究院 | Method for recovering tellurium from tellurium copper slag and preparing high-purity tellurium |
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| JP4016680B2 (en) * | 2002-03-15 | 2007-12-05 | 三菱マテリアル株式会社 | Method for dissolving selenium platinum group element-containing material |
| CN100462453C (en) * | 2007-03-28 | 2009-02-18 | 湖南金旺实业有限公司 | Comprehensive extraction of valent metal from bismuth-containing polymetallic material |
| CN102329966B (en) * | 2011-10-20 | 2013-04-03 | 铜陵有色金属集团股份有限公司 | Wet treatment process of refining slag from Kaldo furnace |
| CN102994766B (en) * | 2012-12-12 | 2014-06-04 | 四会市鸿明贵金属有限公司 | Method for comprehensively recovering valuable metal from copper tellurium slag |
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