CN105925811B - A kind of method that synergistic oxidation leaches tellurium in tellurium slag - Google Patents

A kind of method that synergistic oxidation leaches tellurium in tellurium slag Download PDF

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CN105925811B
CN105925811B CN201610300392.2A CN201610300392A CN105925811B CN 105925811 B CN105925811 B CN 105925811B CN 201610300392 A CN201610300392 A CN 201610300392A CN 105925811 B CN105925811 B CN 105925811B
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tellurium
copper
bismuth
slag
leaching
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CN105925811A (en
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郭学益
许志鹏
李栋
田庆华
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Central South University
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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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/04—Working-up slag
    • 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
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • 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

The invention discloses a kind of method that synergistic oxidation leaches tellurium in tellurium slag, comprise the following steps：(1) sodium chloride is added in sulfuric acid solution, 60~90 DEG C is heated to and is incubated, ozone is then passed to and adds tellurium slag, is stirred；(2) under conditions of being kept stirring for, separation of solid and liquid after hydrogen peroxide, synergy ozone Oxidation Leaching, 2~8h of reaction is passed through into the solution after step (1), leached mud and leachate containing tellurium is obtained.The present invention is using in O3/H2O2Under system, the extremely strong hydroxyl radical free radical of oxidability is produced, using the strong oxidizing property of hydroxyl radical free radical, the rock-steady structure of lead telluride and bismuthic acid copper is opened, make tellurium, bismuth, copper exposure, and the close chlorine characteristic of tellurium and bismuth, make the leaching effect of tellurium in tellurium slag, bismuth, copper good, tellurium leaching rate is up to 99%, bismuth leaching rate is up to 96%, copper leaching rate realizes efficient, the directly leaching of tellurium in complicated tellurium slag, is conducive to the substep of tellurium, bismuth, copper and antimony to reclaim up to 99%.

Description

A kind of method that synergistic oxidation leaches tellurium in tellurium slag
Technical field
The collaboration leaching of tellurium slag is realized the present invention relates to a kind of method that synergistic oxidation leaches tellurium in tellurium slag, more particularly to one kind The Wet-process metallurgy method of enrichment is efficiently separated with valuable metal.
Background technology
Tellurium is a kind of important dissipated metal, due to its special physicochemical properties, is widely used in metallurgical, change Work, oil, electronics, electrically, various fields, the especially tellurides such as glass ceramics, pigment and medicine have the high temperature difference electronic Gesture and good opto-electronic conversion performance so that development of the tellurium in terms of semiconductor refrigerating part and solar energy is particularly rapid.At present, tellurium Association is reclaimed mainly from copper concentrate and lead concentrate, by pyrometallurgical smelting electrolytic refining process in copper concentrate or lead concentrate After reason, tellurium is set to be enriched in the earth of positive pole of electrorefining processes output.The separation-extraction technology of tellurium mainly have sulfating roasting method, Soda roasting method, oxidation acid leaching, alkali oxide leaching, pressurized acid leaching, alkaline pressure of oxygen leaching, chloridising, ion exchange and solvent extraction etc.. Current is industrially alkali leaching and oxidation acid leaching using wider method.
The thing of tellurium is mutually different in tellurium slag, and the method taken is different, when the thing of tellurium in tellurium slag be mainly mutually tellurium dioxide and During sodium tellurite, the method taken is alkaline leaching, this method tellurium Slag treatment effect high to tellurium dioxide and sodium tellurite content It is good, but for the tellurium slag containing llurate and tellurides, this method effect is poor.For the tellurium slag containing llurate and tellurides, The method taken is oxidation acid leaching method, and this method mainly in sulfuric acid medium, is made in llurate and tellurides by oxidant Tellurium enter solution, but during using conventional oxidant oxidation acid leaching, the leaching rate of tellurium uses potassium permanganate to leach less than 80% When, although the leaching rate of tellurium can reach 90%, but introduce foreign ion, increase the later separation recovery difficult of tellurium.
The content of the invention
The problem of existing for prior art, the present invention provides a kind of method that synergistic oxidation leaches tellurium in tellurium slag, we Method has effectively facilitated the leaching of tellurium in tellurium slag, makes copper in tellurium slag, tellurium, bismuth, antimony and lead valuable metal trend rationally and concentrates, favorably In synthetical recovery, energy consumption is both reduced, while having good organic efficiency.
In order to solve the above technical problems, technical scheme proposed by the present invention is：
A kind of method that synergistic oxidation leaches tellurium in tellurium slag, comprises the following steps：
(1) sodium chloride is added in sulfuric acid solution, 60~90 DEG C is heated to and is incubated, ozone is then passed to and adds tellurium Slag, stirring；
(2) under conditions of being kept stirring for, it is passed through hydrogen peroxide into the solution after step (1), synergy ozone Oxidation Leaching, Separation of solid and liquid after 2~8h is reacted, leached mud and leachate containing tellurium is obtained.
Above-mentioned method, it is preferred that in the step (1), the flow for being passed through ozone is 1~2L/min；Sulfuric acid solution Concentration is 2~6mol/L.
Above-mentioned method, it is preferred that in the step (1), the addition quality of sodium chloride for tellurium slag amount 20%~ 50%；The quality and the volume ratio of sulfuric acid solution that tellurium slag is added are 1：(4~8)；Ratio unit is Kg/L.
Above-mentioned method, it is preferred that in the step (1), tellurium slag needs to carry out sieving processing, sieve before sulfuric acid solution is added Aperture be 75~150um.
Above-mentioned method, it is preferred that in the step (2), hydrogen peroxide add volume for sulfuric acid solution volume 20~ 40%.
Above-mentioned method, it is preferred that in the step (2), mixing speed is 200~300r/min；Hydrogen peroxide is to pass through What the rotating speed of control constant flow pump was passed through, the rotating speed of constant flow pump is 10~20r/min.
Above-mentioned method, it is preferred that in the step (2), the leachate containing tellurium reclaims copper, heavy copper first with eddy flow electrodeposition Liquid obtains thick tellurium using sodium sulfite reduction afterwards, and molten build of thick tellurium obtains tellurium ingot；Liquid prepares thick bismuth according to common process after heavy tellurium.
Above-mentioned method, it is preferred that in the step (2), addition vulcanized sodium is obtained containing antimony in obtained leached mud Leachate and leaded leached mud, then reclaim antimony and lead according to common process.
The main chemical reactions that the synergistic oxidation leaching process of the present invention occurs are as follows：
2O3+H2O2→2·OH+3O2 (1)
PbTe+8·OH+4H2SO4+6NaCl→PbSO4+TeCl6+3Na2SO4+8H2O (2)
CuBi2O4+4·OH+6H2SO4+10NaCl→CuSO4+5Na2SO4+2BiCl5+8H2O (3)
The general principle of the present invention：When being passed through ozone in hydrogen peroxide solution, a large amount of very active hydroxyl frees are produced Base (OH)；Hydroxyl radical free radical is a kind of most active bioactive molecule, is also one of offensiveness most strong material, its oxidizing potential Up to 2.80V, it is suitable with the oxidability of fluorine, much larger than other oxidants；The hydroxyl radical free radical of generation is by constitutionally stable tellurium Change lead and the destruction of bismuthic acid copper, make tellurium, bismuth, copper exposure, recycle the close chlorine characteristic of tellurium and bismuth, make in H2SO4Will in/NaCl systems Tellurium, bismuth, copper are leached into solution, and make the enrichment of element such as lead, antimony in slag；Leachate can reclaim copper using eddy flow electrodeposition, sink Liquid obtains thick tellurium using sodium sulfite reduction after copper, and molten build of thick tellurium obtains tellurium ingot；Liquid prepares thick bismuth according to common process after heavy tellurium. Vulcanized sodium is added in leached mud and obtains leachate and leaded leached mud containing antimony, then antimony and lead is reclaimed according to common process.
Compared with prior art, the advantage of the invention is that：
(1) present invention is using in O3/H2O2Under system, the extremely strong hydroxyl radical free radical of oxidability is produced, hydroxyl free is utilized The strong oxidizing property of base, opens the rock-steady structure of lead telluride and bismuthic acid copper, makes tellurium, bismuth, copper exposure, and the close chlorine of tellurium and bismuth special Property, makes the leaching effect of tellurium in tellurium slag, bismuth, copper good, tellurium leaching rate up to 99%, bismuth leaching rate up to 96%, copper leaching rate up to 99%, Efficient, the directly leaching of tellurium in complicated tellurium slag are realized, is conducive to the substep of tellurium, bismuth, copper and antimony to reclaim.
(2) technique of the invention realizes the purposes such as normal pressure is reduced, reduction yield is big, and required reaction condition is simple, reaction Flow is short, effect is good, required reagent and equipment are common hydrometallurgy industrial equipment, overall to be very easy to realize industrialization Production application.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Fig. 2 is the XRD of the leached mud of the embodiment of the present invention 1.
Embodiment
For the ease of understanding the present invention, more complete is made to the present invention below in conjunction with Figure of description and preferred embodiment Face, meticulously describe, but protection scope of the present invention is not limited to embodiment in detail below.
Unless otherwise defined, the implication that all technical terms used hereinafter are generally understood that with those skilled in the art It is identical.Technical term used herein is intended merely to describe the purpose of specific embodiment, is not intended to the limitation present invention Protection domain.
Except there is a special instruction, the various reagents used in the present invention, raw material be can be commercially commodity or Person can pass through product made from known method.
The chemical composition of tellurium slag is shown in Table 1 used by following examples.
The tellurium dreg chemistry of table 1 constitutes table
Embodiment 1：
A kind of method that synergistic oxidation of the invention leaches tellurium in tellurium slag, its process chart is as shown in figure 1, including following Step：
(1) 4.60mol/L sulfuric acid solution is prepared, and adds sodium chloride of the tellurium slag weight than 20%, 90 DEG C is heated to, presses Ozone is passed through according to 1L/min flow, is then 6 by liquid-solid ratio (liquor capacity L and solid masses Kg ratios):1 amount adds mill It is thin that the tellurium slag that aperture is 150 tm screens, leaching are crossed to 100%；
(2) speed is kept stirring for for 300r/min, and adds sulfuric acid volume by controlling constant flow pump 10r/min speed 20% concentration is the progress of 30% hydrogen peroxide synergistic oxidation reaction, reacts 5h, has reacted the realization of use vacuum filtration mode Solid-liquor separation, obtain leached mud (XRD spectrum is shown in Fig. 2) containing antimony and lead and containing tellurium, bismuth, copper leachate.The process tellurium soaks Go out up to 98.96%, bismuth leaching rate is up to 98.58%, and copper leaching rate is up to 99.79%.
(3) leachate is reclaimed liquid after copper, heavy copper first with eddy flow electrodeposition process and then obtained using sodium sulfite reduction Thick tellurium, finally melts to build and obtains tellurium ingot, and liquid prepares thick bismuth according to common process after heavy tellurium；Leached mud is leached using vulcanized sodium and realizes antimony With the separation of lead, then antimony is reclaimed according to common process.
Embodiment 2：
A kind of method that synergistic oxidation of the invention leaches tellurium in tellurium slag, its process chart is as shown in figure 1, including following Step：
(1) 3.68mol/L sulfuric acid solution is prepared, and adds sodium chloride of the tellurium slag weight than 25%, 85 DEG C is heated to, presses Ozone is passed through according to 2L/min, then by liquid-solid ratio (liquor capacity L and solid masses Kg ratios) 7:1 amount addition is levigate extremely 100% crosses the tellurium slag that aperture is 100 tm screens, leaching；
(2) speed 300r/min is kept stirring for, and sulfuric acid volume 25% is added by controlling constant flow pump 20r/min speed Concentration be progress that 30% hydrogen peroxide synergistic oxidation reacts, reaction time 7h reacted use vacuum filtration mode and realized liquid Gu separation, obtain leached mud containing antimony and lead and containing tellurium, bismuth, copper leachate.The process tellurium is leached up to 97.65%, bismuth leaching Extracting rate is up to 96.32%, and copper leaching rate is up to 99.65%.
(3) leachate containing tellurium, bismuth, copper reclaims after copper, heavy copper liquid first with eddy flow electrodeposition and then utilizes sodium sulfite Reduction obtains thick tellurium, and finally molten build obtains tellurium ingot, and liquid prepares thick bismuth according to common process after heavy tellurium；Leached mud then utilizes vulcanized sodium The separation for realizing antimony and lead is leached, then antimony is reclaimed according to common process.
Embodiment 3：
A kind of method that synergistic oxidation of the invention leaches tellurium in tellurium slag, its process chart is as shown in figure 1, including following Step：
(1) 2.76mol/L sulfuric acid solution is prepared, and adds sodium chloride of the tellurium slag weight than 30%, 80 DEG C is heated to, presses Ozone is passed through according to 2L/min flow, then by liquid-solid ratio (liquor capacity L and solid masses Kg ratios) 8:1 addition is levigate extremely 100% crosses the tellurium slag that aperture is 75 tm screens, leaching；
(2) speed 300r/min is kept stirring for, and sulfuric acid volume 30% is added by controlling constant flow pump 15r/min speed Concentration for 30% hydrogen peroxide synergistic oxidation react progress, reaction time 8h, react use vacuum filtration mode realize Solid-liquor separation, obtain leached mud containing antimony and lead and containing tellurium, bismuth, copper leachate.The process tellurium is leached up to 96.82%, bismuth Leaching rate is up to 94.54%, and copper leaching rate is up to 99.33%.
(3) containing tellurium, bismuth, copper leachate first with eddy flow electrodeposition process reclaim copper, sink copper after liquid using sodium sulfite also Original obtains thick tellurium, and finally molten build obtains tellurium ingot, and liquid prepares thick bismuth according to common process after heavy tellurium；Leached mud is then soaked using vulcanized sodium Go out to realize the separation of antimony and lead, then reclaim antimony according to common process.
Comparative example 1：
The method of this comparative example tellurium oxide from tellurium slag is leached, comprises the following steps：
(1) 5.0mol/L sulfuric acid solution is prepared, and adds sodium chloride of the tellurium slag weight than 20%, 80 DEG C is heated to, presses Ozone is passed through according to 2L/min flow, is then 10 by liquid-solid ratio (liquor capacity L and solid masses Kg ratios):1 amount is added It is levigate that the tellurium slag that aperture is 150 tm screens, leaching are crossed to 100%；
(2) speed is kept stirring for for 300r/min, reaction time 6h, has been reacted use vacuum filtration mode and has been realized that liquid divides admittedly From, obtain leached mud containing antimony and lead and containing tellurium, bismuth, copper leachate.The process tellurium leaching rate is only 28.24%, bismuth leaching Extracting rate is up to 9.418%, and copper leaching rate is up to 67.75%.
Comparative example 2：
The method of this comparative example tellurium oxide from tellurium slag is leached, comprises the following steps：
(1) 5.0mol/L sulfuric acid solution is prepared, and adds sodium chloride of the tellurium slag weight than 20%, 80 DEG C is heated to, leads to The hydrogen peroxide that the concentration for the speed addition sulfuric acid solution volume 20% for controlling constant flow pump 15r/min is 30% is crossed, it is then solid by liquid It is 10 than (liquor capacity L and solid masses Kg ratios):1 amount addition is levigate to cross the tellurium that aperture is 150 tm screens to 100% Slag, leaching；
(2) speed is kept stirring for for 300r/min, reaction time 6h, has been reacted use vacuum filtration mode and has been realized that liquid divides admittedly From, obtain leached mud containing antimony and lead and containing tellurium, bismuth, copper leachate.The process tellurium leaching rate is only 15.75%, bismuth leaching Extracting rate is up to 1.65%, and copper leaching rate is up to 56.37%.
From embodiment 1-3 and comparative example 1-2 Comparison of experiment results, the present invention is in O3/H2O2Synergy under, The extremely strong hydroxyl radical free radical of oxidability is produced, using the strong oxidizing property of hydroxyl radical free radical, the steady of lead telluride and bismuthic acid copper is opened Fixed structure, makes the close chlorine characteristic of tellurium, bismuth, copper exposure, and tellurium and bismuth, makes the leaching effect of tellurium in tellurium slag, bismuth, copper good, tellurium leaching Extracting rate is up to 99%, and bismuth leaching rate is up to 96%, and copper leaching rate realizes efficient, the directly leaching of tellurium in complicated tellurium slag, favorably up to 99% Reclaimed in the substep of tellurium, bismuth, copper and antimony.

Claims (4)

1. a kind of method that synergistic oxidation leaches tellurium in tellurium slag, it is characterised in that comprise the following steps：
(1) sodium chloride is added in sulfuric acid solution, 60~90 DEG C is heated to and is incubated, ozone is then passed to and adds tellurium slag, stir Mix；Wherein, the flow for being passed through ozone is 1~2L/min；The concentration of sulfuric acid solution is 2~6mol/L；The addition quality of sodium chloride For the 20%~50% of tellurium slag amount；The quality and the volume ratio of sulfuric acid solution that tellurium slag is added are 1：(4~8)；Ratio unit For Kg/L；
(2) under conditions of being kept stirring for, hydrogen peroxide, synergy ozone Oxidation Leaching, reaction are passed through into the solution after step (1) Separation of solid and liquid after 2~8h, obtain leached mud and containing tellurium, bismuth, copper leachate；Wherein, the volume that hydrogen peroxide is added is molten for sulfuric acid The 20%~40% of liquid product；Mixing speed is 200~300r/min；Hydrogen peroxide is passed through by controlling the rotating speed of constant flow pump , the rotating speed of constant flow pump is 10~20r/min.
2. the method as described in claim 1, it is characterised in that in the step (1), tellurium slag needed before sulfuric acid solution is added into Row sieving is handled, and the aperture of sieve is 75~150um.
3. method as claimed in claim 1 or 2, it is characterised in that in the step (2), the leachate containing tellurium, bismuth, copper is first Liquid after copper, heavy copper being reclaimed using eddy flow electrodeposition thick tellurium being obtained using sodium sulfite reduction, molten build of thick tellurium obtains tellurium ingot；Liquid after heavy tellurium Thick bismuth is prepared according to common process.
4. method as claimed in claim 1 or 2, it is characterised in that in the step (2), is added in obtained leached mud Vulcanized sodium obtains leachate and leaded leached mud containing antimony, then reclaims antimony and lead according to common process.
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CN106636661B (en) * 2016-12-15 2018-06-26 中南大学 A kind of method of Selective Separation recycling tellurium and antimony in slag from tellurium
CN107312932B (en) * 2017-06-22 2019-03-05 中南大学 A kind of method that separate precious metal is enriched with valuable metal in material
CN110396597A (en) * 2019-07-19 2019-11-01 江西铜业集团有限公司 A kind of selecting smelting combination process of the high efficiency extraction lead bismuth from oxidation cleaning residue
CN113564374A (en) * 2021-07-28 2021-10-29 云南驰宏资源综合利用有限公司 Method for producing coarse copper powder from copper-bismuth slag
CN113564622B (en) * 2021-08-09 2022-10-28 安徽工业大学 Method for efficiently separating copper and tellurium from copper telluride material

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US7731920B2 (en) * 2005-06-03 2010-06-08 Brookhaven Science Associates System and method for separating tellurium from cadmium waste
CN101508426B (en) * 2009-03-24 2010-12-29 中南大学 Method for separating tellurium from tellurium slag
CN102390819B (en) * 2011-08-10 2013-04-10 辽宁大学 Method for preparing tellurium dioxide from tellurium slag
CN103194617B (en) * 2013-04-23 2014-01-15 昆明理工大学 Method for strengthening agitation leaching of cuprite red copper ore type copper oxide
CN105112668B (en) * 2015-09-02 2017-04-12 中南大学 Method for separating and enriching valuable metals from copper anode mud

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