CN102745657B - Method for extracting tellurium from tellurium copper slags - Google Patents
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Abstract
The invention provides a method for extracting tellurium from tellurium copper slags. The method includes the following steps of (1) sulfating calcination at a high temperature, grinding the tellurium copper slags, mixing ground tellurium copper slags with a concentrated sulfuric acid to calcine, enabling the mass ratio between the concentrated sulfuric acid and the tellurium copper slags to be (1.2-1.5):1, maintaining the calcination temperature in a range from 450 DEG C to 600 DEG C and maintaining the calcination time in a range from 3 hours to 5 hours; (2) alkaline leaching to separate the tellurium, leaching obtained calcination slags by a sodium hydroxide alkaline liquor, and then filtering to obtain a tellurium containing alkali leaching liquid and alkali leaching slags; (3) oxidizing the alkali leaching liquid, oxidizing the tellurium containing alkali leaching liquid by sodium hypochlorite of an oxidant and then filtering to obtain sodium tellurate filtered slags; and (4) acid dissolution reduction, dissolving the sodium tellurate filtered slags by a chloridion containing acidic system, adding a reducing agent to achieve reduction and then filtering to obtain tellurium powders. According to the method for extracting the tellurium from the tellurium copper slags, a complete separation of copper, selenium and tellurium can be fully achieved, a comprehensive recovery of the copper, selenium and tellurium can be achieved, the technological process is simple, tellurium dioxide of an intermediate product is not required, the tellurium powders with a high purity can be directly produced, and the tellurium powders can serve as raw materials of 6N high purity tellurium.
Description
Technical field
The present invention relates to non-ferrous metal metallurgy technical field, be specifically related to a kind of method of extracting tellurium from tellurium copper slag.
Background technology
Along with development in science and technology, rare elements tellurium has become the required important materials of industry development such as robot calculator, communication, aerospace, the energy, medical and health.Tellurium is very low at occurring in nature content, seldom has independent ore deposit, and main association is in chalcopyrite.Copper anode mud pyrorefining soda slag (being commonly called as Cao Da slag) is the main raw material that traditional industry is extracted tellurium.In copper anode mud pyrorefining process, sodium carbonate is combined with telluride and is generated soda slag, and in soda slag, chief component material is Na
2cO
3, NaO, Na
2teO
3, due to Na
2teO
3soluble in water, generally adopt that water logging+alkali soaks, removal of impurities, electrodeposition process carry tellurium from soda slag.
Copper anode mud oxygen presses leaching decopper(ing) novel process to have the features such as decopper(ing) efficiency is high, environmental protection is good, is adopted gradually by copper anode mud processing enterprise.Copper anode mud oxygen press to leach when decopper(ing) technique leaches copper can leach tellurium, output byproduct tellurium copper slag.Tellurium copper slag principal goods phase composite: copper exists with elemental copper and cuprous telluride form, tellurium is that cuprous telluride form exists, valence state is-divalent that selenium is simple substance selenium.Tellurium copper slag principal constituent (mass percent): Cu 30-60%, Te 15-30%, Se1-5%, Bi 0.1-0.3%, Sb 0.01-0.1%.
Tellurium copper slag system is complicated containing tellurium material, the treatment process core of this material is to the complete separation of copper, selenium, three kinds of principal elements of tellurium.Because tellurium in tellurium copper slag is-divalent tellurium copper compound but not 4 valency tellurium oxide compounds, under normal pressure, not by leaching with sodium hydroxide, traditional soda slag alkali soaking technology cannot be processed tellurium copper slag.There is the alkaline condition that is treated to of bibliographical information cuprous telluride to lead to oxygen pressure leaching process, this art breading tellurium copper slag exists tellurium to be easily oxidized the 6 valency telluriums that excessive generation is insoluble in alkali, the shortcoming that causes the tellurium rate of recovery to reduce, and this technique must use high-tension apparatus, has certain potential safety hazard.Some bibliographical information peracidity condition Oxidation Leachings are containing the technique of tellurium material, and this type of technique is mainly confined to copper, tellurium separation or selenium, tellurium is separated, cannot accomplish that copper, selenium, three kinds of elements of tellurium are entirely separated completely.
Application number be 201110449606.X patent report a kind of novel process of processing tellurium slag, this art breading object is that soda pulp water soaks the indissoluble tellurium slag after filtration, this Technology core is the acidizing fired separating copper of Sulfur-Vapor of Lower Temperature, tellurium, and maturing temperature is 150 ℃-250 ℃.But this technique is not suitable for the processing of the slag of tellurium copper described in literary composition, major cause: one, this technique cannot solve the selenium problem separated with tellurium copper, because this technique maturing temperature (top temperature is 250 ℃) is lower than 335 ℃ of the minimum temperatures of seleno oxide volatilization, cannot selenium is separated with tellurium copper; Two, this art breading tellurium copper slag roasting effect is poor, in tellurium copper slag, tellurium all exists with cuprous telluride form, Chemical bond ability is more intense, and it is higher that cuprous telluride accounts for material gross weight ratio, under cold condition, sulfurization roasting degree of oxidation is inadequate, according to contriver's experimental result, show, lower than 400 ℃, after the sulfurization roasting of tellurium copper slag, the leaching yield of tellurium is lower than 50%.Application number is that 201110344761.5 patent has proposed oxidation, reduction and processes the technique that the alkali immersion liquid of tellurium obtains tellurium dioxide, this process using hydrogen peroxide is made oxygenant, hydrogen peroxide easily decomposes under alkaline condition causes that oxidation efficiency is not high, reagent consumption is large, and hydrogen peroxide consumption is generally doubly theoretical consumption of 6-8 in actual applications; Reduction output tellurium dioxide process is difficult to control when practical application, and I haven't seen you for ages causes the tellurium rate of recovery to reduce for S-WAT add-on, and the large generation simple substance tellurium of S-WAT add-on affects the quality of tellurium dioxide.Above two patents are all to take soda slag as processing object, with the form of tellurium dioxide, extract tellurium, and follow-up, removal of impurities molten according to common process alkali, electrodeposition are carried tellurium, and this type of technical process is complicated, and the cycle is long.
Summary of the invention
The problem that the present invention solves is to provide a kind of method of extracting tellurium from tellurium copper slag, makes copper, selenium, tellurium thoroughly separated, and reaches copper, selenium, the comprehensive object reclaiming of tellurium.
In order to solve the problems of the technologies described above, technical scheme of the present invention is:
A method of extracting tellurium from tellurium copper slag, comprises the following steps:
(1) high-temperature sulfuric acid roasting
Tellurium copper sizing is broken, mix with the vitriol oil, mixture carries out roasting, roasting condition: the vitriol oil and tellurium copper slag mass ratio are 1.2-1.5: 1,450 ℃-600 ℃ of maturing temperatures, roasting time 3h-5h;
(2) alkali soaks a minute tellurium
With sodium hydroxide lye, leach the fired slags obtaining, filter after completion of the reaction, obtain alkali and soak slag and contain the immersion liquid of tellurium alkali;
(3) alkali immersion liquid oxidation
Described in employing oxygenant hypochlorite oxidation, containing the immersion liquid of tellurium alkali, filter after completion of the reaction, obtain sodium tellurate filter residue;
(4) sour molten reduction
After described sodium tellurate filter residue being dissolved with chloride ion-containing acid system, add reductive agent reduction, filter after completion of the reaction, obtain tellurium powder.
As preferably, in described (2), NaOH concentration is 2mol/L-4mol/L, 70 ℃-90 ℃ of temperature of reaction, and the mass ratio of described NaOH alkali lye and described fired slags is 5-8: 1, reaction times 3h-5h.
As preferably, in described (3), NaClO add-on is required theoretical amount of substance 1.1 times-1.5 times, 40 ℃-60 ℃ of temperature of reaction, reaction times 3h-5h.
As preferably, in described (4), chlorion and the hydrogen ion concentration of chloride ion-containing acid system are 5mol/L-8mol/L, and the mass ratio of chloride ion-containing acid system and described sodium tellurate filter residue is 5-9: 1.
As preferably, described chloride ion-containing acid system is hydrochloric acid, or the mixture of sulfuric acid and sodium-chlor.
As preferably, described chloride ion-containing acid system is hydrochloric acid.
As preferably, in described (4), reductive agent consumption is required theoretical amount of substance 1 times-6 times, 60 ℃-90 ℃ of reduction reaction temperatures, reaction times 2h-4h.
As preferably, described reductive agent is sulphite or sulfurous gas.
As preferably, described reductive agent is S-WAT.
The present invention is according to tellurium copper slag material feature, and specific aim proposes high-temperature sulfuric acid roasting tellurium copper slag, and fully, selenium is separated with tellurium copper and reclaimed selenium good separating effect in material oxidation; Alkali soaks fired slags and leaches tellurium, makes copper tellurium separated, and alkali soaks the recyclable copper of slag; Containing the immersion liquid of tellurium alkali, through oxidation, generate sodium tellurate precipitation, further separated with impurity; With chloride acid system, dissolve sodium tellurate, reductive agent reduction generates tellurium powder.Whole technique fully realizes the complete separation of copper, selenium, tellurium, and accomplishes that three kinds of elements comprehensively reclaim, and flow process is simple, and without intermediates tellurium dioxide, the direct higher tellurium powder of output purity, can be used as the raw materials for production of 6N high purity tellurium.
Accompanying drawing explanation
Fig. 1 extracts the process schematic representation of tellurium for what a kind of embodiment of the present invention provided from tellurium copper slag.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these are described is for further illustrating the features and advantages of the present invention, rather than limiting to the claimed invention.
The invention provides a kind of method of extracting tellurium from tellurium copper slag, its step please refer to Fig. 1, and Fig. 1 extracts the process schematic representation of tellurium for what a kind of embodiment of the present invention provided from tellurium copper slag.
The invention provides a kind of method of extracting tellurium from tellurium copper slag, comprise the following steps:
(1) high-temperature sulfuric acid roasting
Preferably tellurium copper sizing is broken to and is not less than 100 orders, mix with the vitriol oil, the vitriol oil is that mass concentration is more than or equal to 70% sulphuric acid soln, roasting under mixture high temperature, roasting condition: the vitriol oil and tellurium copper slag mass ratio are 1.2-1.5: 1,450 ℃-600 ℃ of maturing temperatures, roasting time 3-5h, then wash the recyclable thick selenium of baking flue gas with water, fired slags is crushed to and is not less than 100 orders.
There is following reaction in high-temperature sulfuric acid roasting:
Se+2H
2SO
4＝SeO
2+2SO
2+2H
2O
Cu
2Te+6H
2SO
4＝2CuSO
4+TeO
2+4SO
2+6H
2O
Cu+2H
2SO
4＝CuSO
4+SO
2+2H
2O
Thick selenium reclaims reaction:
SeO
2+H
2O＝H
2SeO
3
H
2SeO
3+2SO
2+H
2O＝Se+2H
2SO
4
In order to guarantee sulfurization roasting oxidation effectiveness, two processing parameters are more crucial: the one, and the vitriol oil and tellurium copper slag mass ratio need be controlled at 1.2-1.5: 1, it is the twice of sulfuric acid consumption in the patent of 201110449606.X, avoid because vitriol oil amount is few, the insufficient tellurium roasting effect that causes of material oxidation is poor, and the alkali that affects tellurium soaks efficiency; The 2nd, control reasonable maturing temperature scope, in order to guarantee the abundant voloxidation of selenium, maturing temperature is not less than 450 ℃, but can not surpass 600 ℃, thereby otherwise excess Temperature tellurium oxide can volatilize and reduce the rate of recovery of tellurium.
(2) alkali soaks a minute tellurium
With sodium hydroxide lye, leach fired slags, preferably NaOH concentration is that the mass ratio of 2mol/L-4mol/L, 70 ℃-90 ℃ of temperature of reaction, NaOH alkali lye and described fired slags is 5-8, reaction times 3h-5h.Filter after completion of the reaction, alkali soaks slag for reclaiming copper, containing the immersion liquid of tellurium alkali, enters next step processing.
Alkali soaks reaction:
TeO
2+2NaOH＝Na
2TeO
3+H
2O
CuSO
4+2NaOH＝Cu(OH)
2+Na
2SO
4
In fired slags, copper is vitriol, generates insolubles copper hydroxide under alkaline condition, and in slag, tellurium oxide is combined with sodium hydroxide and is generated sodium tellurite lyotrope, thereby reaches the completely separated of copper and tellurium.
(3) alkali immersion liquid oxidation
Adopt oxygenant hypochlorite oxidation containing the immersion liquid of tellurium alkali, 1.1 times-1.5 times (required theoretical amount of substance is shown in following reaction formula) that preferably NaClO add-on is required theoretical amount of substance, 40 ℃-60 ℃ of temperature of reaction, reaction times 3h-5h, filter after completion of the reaction, obtain sodium tellurate filter residue, filtrate can be for leaching fired slags after hydrogen make-up sodium oxide.
Oxidizing reaction:
Na
2TeO
3+NaClO＝Na
2TeO
4+NaCl
Owing to being dissolved with a small amount of arsenic, selenium element containing in the immersion liquid of tellurium alkali, in order further tellurium to be carried out separated with impurity element especially selenium, utilize clorox that sodium tellurite is oxidized to sodium tellurate, sodium tellurate is insolubles at alkaline condition, and arsenic impurities, selenium element are not affected by valence state at alkaline condition, it is all lyotrope, thereby make tellurium further separated with arsenic, selenium, for the follow-up higher-grade simple substance tellurium that obtains creates conditions.In addition select clorox to make oxygenant, mainly consider that clorox oxidation susceptibility under alkaline condition is very strong, and more stable under alkaline condition, being not easy to decompose, in oxidising process, utilization ratio is high, consumes few.
(4) sour molten reduction
After sodium tellurate filter residue being dissolved with chloride ion-containing acid system, add reductive agent reduction, filter after completion of the reaction, obtain tellurium powder.
Wherein the chlorion of chloride ion-containing acid system and hydrogen ion concentration are 5mol/L-8mol/L, the mass ratio of chloride ion-containing acid system and sodium tellurate filter residue is 5-9: 1, this chloride ion-containing acid system can be selected hydrochloric acid, or the mixture of sulfuric acid and sodium-chlor, preferably uses hydrochloric acid; Reductive agent consumption is 1 times-6 times (required theoretical amount of substance is shown in following reaction formula) of required theoretical amount of substance, 60 ℃-90 ℃ of reduction reaction temperatures, reaction times 2h-4h, this reductive agent can be selected sulphite or sulfurous gas, preferably uses S-WAT.
The molten reduction reaction of acid (hydrochloric acid of take is example as sour solvent, S-WAT as reductive agent):
Na
2TeO
4+2HCl＝Na
2TeO
3+Cl
2+H
2O
Na
2TeO
3+2Na
2SO
3+2HCl＝2Na
2SO
4+Te+2NaCl+H
2O
In the molten reduction process of acid, chloride acid system has two effects, and one provides sour environment to dissolve sodium tellurate, and its two chlorions reductive tellurium acid sodium generates intermediate product sodium tellurite.Sodium tellurite has stronger oxidisability and is generated simple substance tellurium by S-WAT reduction reaction.The impurity containing due to sodium tellurate is extremely low, and the simple substance tellurium product bit comparison that reduction obtains is high, and especially selenium content is extremely low, is well suited for as the raw material of producing 6N high purity tellurium.
Embodiment 1:
(1) high-temperature sulfuric acid roasting
Get tellurium copper slag 1kg levigate to 100 orders, tellurium copper slag ingredient: Te 20.34%, Cu 52.6%, Se 3.01%, As 0.64%, Bi 0.12%, Sb 0.07%, add the vitriol oil of 1.3kg to stir, start roasting operation, 500 ℃ of maturing temperatures, roasting time 4h, obtains 1.28kg calcining after cooling, calcining is milled to 100 orders, and calcining main component is: Te 15.87%, Cu 41.09%, Se 0.51%, As 0.48%, Bi 0.05%, Sb 0.02%.The flue gas producing in roasting process reclaims selenium by washing spray column, and thick selenium selenium content is 82%.
(2) alkali soaks a minute tellurium
Get the calcining 1.28kg that step (1) obtains, press liquid-solid ratio 7: 1, adding concentration is the sodium hydroxide of 2mol/L, and extraction temperature is 80 ℃, leaches 4h: filter, obtain alkali immersion liquid, alkali immersion liquid composition: Te 21.75g/L, Cu 2.09mg/L, Se 0.65g/L, As 0.47g/L, Bi 0.04g/L.Therefore Te leaching yield is 95.94% when alkali soaks.Alkali soaks after slag is dried and is weighed as 814.82g, and alkali soaks slag ingredient: Cu 64.25%, and Te 1.01%, and Se 0.086%, and when alkali soaks, 99.47% Cu enters in slag.Alkali soaks slag and can adopt ordinary method to reclaim copper.
(3) alkali immersion liquid oxidation
Get that step (2) obtains containing the immersion liquid of tellurium alkali, add the clorox of 1.2 times of theoretical consumptions, extraction temperature is 50 ℃, oxidization time 4h, reacts complete filtration, liquid main component after filter: Te 132mg/L, Cu < 0.5mg/L, Se 562mg/L, As 402mg/L.Oxidation sludge weighs as 348.2g after drying, and its main component is sodium tellurate, and Te content is 53.22%.
(4) sour molten reduction
The oxidation sludge that adds step (3) to obtain in 2.1L hydrochloric acid soln, concentration of hydrochloric acid is 7mol/L, after oxidation sludge is fully sour molten, then adds 750g S-WAT, 70 ℃ of temperature of reaction, reaction times 4h.Filter after completion of the reaction, washing, drying and obtaining 184.8g purity is 99.92% tellurium powder, tellurium powder foreign matter content: Se 0.004%, Cu 0.02%, and As 0.001%.Liquid composition after heavy tellurium: Te 33.06mg/L, Cu < 0.5mg/L, Se 1.21mg/L, As 6.16mg/L.
Embodiment 2:
(1) high-temperature sulfuric acid roasting
Get tellurium copper slag 1kg levigate to 110 orders, tellurium copper slag ingredient: Te 25.73%, Cu 46.66%, Se 2.65%, As 0.58%, Bi 0.11%, Sb 0.08%1Kg, add the vitriol oil of 1.4kg to stir, start roasting operation, 550 ℃ of maturing temperatures, roasting time 5h, obtains 1.32kg calcining after cooling, calcining is milled to 120 orders, and calcining main component is: Te 19.48%, Cu 35.32%, Se 0.46%, As 0.40%, Bi 0.08%, Sb 0.03%.The flue gas producing in roasting process reclaims selenium by washing spray column, alkali lye spray column, and thick selenium selenium content is 80%.
(2) alkali soaks a minute tellurium
Get the calcining 1.32kg that step (1) obtains, press liquid-solid ratio 7: 1, adding concentration is the sodium hydroxide of 3mol/L, and extraction temperature is 90 ℃, leach 4h: filter, obtain alkali immersion liquid, alkali immersion liquid composition: Te 27.26g/L, Cu 1.47mg/L, Se 0.63g/L, As 0.45g/L, Bi 0.02g/L, therefore Te leaching yield is 97.96% when alkali soaks.Alkali soaks after slag is dried and is weighed as 745.2g, and alkali soaks slag ingredient: Cu 61.53%, and Te 0.70%, and Se 0.033%, and when alkali soaks, 98.37% Cu enters in slag.Alkali soaks slag technology recovery copper routinely.
(3) alkali immersion liquid oxidation
Get that step (2) obtains containing the immersion liquid of tellurium alkali, add the clorox of 1.1 times of theoretical consumptions, extraction temperature is 60 ℃, oxidation 4h, filter, obtain oxidated solution, its main component: Te 96mg/L, Cu < 0.5mg/L, Se 581mg/L, As 369mg/L.Oxidation sludge weighs as 458.6g after drying, and its main component is sodium tellurate, and Te content is 52.86%.
(4) sour molten reduction
The oxidation sludge that adds step (3) to obtain in 3.2L sulfuric acid and sodium-chlor mixing solutions, in mixed solution, hydrogen ion and chlorine ion concentration are all 6mol/L, oxidation sludge is after fully sour molten, solution is heated to 80 ℃, add 970g S-WAT, reduction 3h, after completion of the reaction, filter, residue washing, drying and obtaining 242.1g purity is 99.9% tellurium powder, tellurium powder foreign matter content: Se0.001%, Cu 0.01%, and As 0.001%.Liquid composition after heavy tellurium: Te 12.46mg/L, Cu < 0.5mg/L, Se 0.13mg/L, As 1.78mg/L.
Above a kind of method of extracting tellurium from tellurium copper slag provided by the present invention is described in detail.Applied specific case herein principle of the present invention and embodiment are set forth, the explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
Claims (9)
1. from tellurium copper slag, extract a method for tellurium, it is characterized in that, comprise the following steps: (1) high-temperature sulfuric acid roasting
Tellurium copper sizing is broken, mix with the vitriol oil, mixture carries out roasting, roasting condition: the vitriol oil and tellurium copper slag mass ratio are 1.2-1.5:1,450 ℃-600 ℃ of maturing temperatures, roasting time 3h-5h; The described vitriol oil is that mass concentration is more than or equal to 70% sulphuric acid soln;
(2) alkali soaks a minute tellurium
With sodium hydroxide lye, leach the fired slags obtaining, filter after completion of the reaction, obtain alkali and soak slag and contain the immersion liquid of tellurium alkali;
(3) alkali immersion liquid oxidation
Described in employing oxygenant hypochlorite oxidation, containing the immersion liquid of tellurium alkali, filter after completion of the reaction, obtain sodium tellurate filter residue;
(4) sour molten reduction
After described sodium tellurate filter residue being dissolved with chloride ion-containing acid system, add reductive agent reduction, filter after completion of the reaction, obtain tellurium powder.
2. method according to claim 1, is characterized in that, in described (2), NaOH concentration is 2mol/L-4mol/L, 70 ℃-90 ℃ of temperature of reaction, and the mass ratio of described NaOH alkali lye and described fired slags is 5-8:1, reaction times 3h-5h.
3. method according to claim 1, is characterized in that, NaClO add-on is required theoretical amount of substance in described (3) 1.1 times-1.5 times, 40 ℃-60 ℃ of temperature of reaction, reaction times 3h-5h.
4. method according to claim 1, is characterized in that, in described (4), chlorion and the hydrogen ion concentration of chloride ion-containing acid system are 5mol/L-8mol/L, and the mass ratio of chloride ion-containing acid system and described sodium tellurate filter residue is 5-9:1.
5. according to the method described in claim 1 or 4, it is characterized in that, described chloride ion-containing acid system is hydrochloric acid, or the mixture of sulfuric acid and sodium-chlor.
6. method according to claim 5, is characterized in that, described chloride ion-containing acid system is hydrochloric acid.
7. method according to claim 1, is characterized in that, reductive agent consumption is required theoretical amount of substance in described (4) 1 times-6 times, 60 ℃-90 ℃ of reduction reaction temperatures, reaction times 2h-4h.
8. according to the method described in claim 1 or 7, it is characterized in that, described reductive agent is sulphite or sulfurous gas.
9. method according to claim 8, is characterized in that, described reductive agent is S-WAT.
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| CN110255509B (en) * | 2019-07-22 | 2021-02-12 | 阳谷祥光铜业有限公司 | Process for preparing tellurium dioxide |
| CN113697778B (en) * | 2021-08-20 | 2023-12-26 | 金隆铜业有限公司 | Copper tellurium slag treatment method |
| CN115449637B (en) * | 2022-10-14 | 2024-04-19 | 江西理工大学 | Method for efficiently and stepwise separating and extracting selenium, copper and tellurium from copper anode slime |
| CN116281885B (en) * | 2023-04-20 | 2024-04-16 | 赤峰云铜有色金属有限公司 | Device and method for recycling tellurium in copper anode slime |
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| CN101508426B (en) * | 2009-03-24 | 2010-12-29 | 中南大学 | Method for separating tellurium from tellurium slag |
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