CN105506280A - Activation leaching method of strengthened leaching tellurium residues - Google Patents
Activation leaching method of strengthened leaching tellurium residues Download PDFInfo
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- CN105506280A CN105506280A CN201510984362.3A CN201510984362A CN105506280A CN 105506280 A CN105506280 A CN 105506280A CN 201510984362 A CN201510984362 A CN 201510984362A CN 105506280 A CN105506280 A CN 105506280A
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- tellurium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses an activation leaching method of strengthened leaching tellurium residues. The activation leaching method comprises the steps of slurrying the strengthened leaching tellurium residues according to certain liquid-solid ratio; adding the slurry strengthened leaching tellurium residues into a ball mill; adding sodium hydroxide and sodium sulfide with the required weight at the same time; adding grinding balls according to the required ball-to-powder weight ratio; starting the ball mill; carrying out reaction for certain time under a prescribed ball milling system; reacting undissolved tellurite or tellurate with sodium sulfide; dissolving generated Na2TeO3 in a solution; generating MeS sediment through heavy metals, and feeding the MeS sediment into the leaching residues; after ball milling, carrying out solid-liquid separation on the mixed slurry through directly adopting vacuum filtration; preparing tellurium ingots with a leaching solution according to a traditional technology; and recycling other valuable metals in the leaching residues. According to the method, the strengthened leaching tellurium residues are fully dissolved in an alkaline sodium sulfide solution through ball milling activation, the leaching rate of tellurium in the strengthened leaching tellurium residues can be increased to 75.0% or above, and the method has the advantages of high leaching rate and simple operation.
Description
Technical field the present invention relates to hydrometallurgy process in nonferrous metallurgy field, particularly effectively realizes the Wet-process metallurgy method that the activation of tellurium slag Strengthen education slag is leached.
Background technology tellurium is period 5 VI B race element in the periodic table of elements, symbol of element Te (English Tellurium), tellurium is one of important dissipated metal, due to the physicochemical property that it is special, be widely used in metallurgy, chemical industry, oil, electronics, electrically, the various fields such as glass-ceramic, pigment and medicine, especially telluride has high thermoelectromotive force and good opto-electronic conversion performance, the application of tellurium in semiconductor refrigerating part and sun power has been had and develops rapidly.80% of tellurium consumption is applied to metallurgical industry, 80% of tellurium consumption be in metallurgical industry apply (Zhou Lingzhi. dissipated metal handbook. press of Central South University, 1993.): steel and copper alloy add a small amount of tellurium, its machinability can be improved and increase hardness; In white cast iron, tellurium is used as carbide stabilizer, makes hard-surface wear-resisting.
The mineral deposit of tellurium mainly contains independent deposit and accompanying mineral deposit, wherein in independent deposit, tellurium mainly exists with tetradymite, and in accompanying mineral deposit, mainly containing porphyry copper, rock copper mine, chalcopyrite, lead glance and precious metal ore etc., current most of tellurium extracts in the by product by non-ferrous metal copper and plumbous smelting process.The copper ore concentrates of association tellurium or lead ore concentrate are through pyrometallurgical smelting-pyrorefining and electrolytic refining process output cathode copper or cathode lead, make simultaneously tellurium to be enriched in the by product anode sludge of electrorefining processes (poplar natural feet precious metals metallurgy and product deep processing. press of Central South University, 2005.).Copper anode mud and lead anode slurry are the important source material extracting tellurium, in copper anode mud and lead anode slurry, tellurium content is respectively 0.5 ~ 5.09% and 0.01 ~ 0.9%, can find out, in copper anode mud, tellurium content is than high in lead anode slurry, and the extracting method of tellurium has very big-difference according to anode slime treatment process difference.
The treatment process of the anode sludge mainly comprises pre-treatment, enrichment and refining three links, wherein the enriched substance of tellurium is mainly from pre-treatment and these two link outputs of enrichment, because the treatment process adopted is different, the enriched product of tellurium is had nothing in common with each other (Peng Rongqiu, the comprehensive utilization of heavy metal metallurgy factories. press of Central South University, 2006).Tellurium in copper anode mud is two part outputs, one is with the form output of telluride copper at preprocessing process, two is with tellurium slag form output in pyrometallurgical smelting process, and the tellurium in lead anode slurry in pyrometallurgical smelting technique with tellurium slag form output, so tellurium slag is the most important tellurium enriched substance of anode sludge pyrogenic attack technological process, also known as soda slag, main containing Te, Na, Bi, Cu, Pb, Ag, Se, the elements such as As and Sb, containing free sodium carbonate or sodium oxide in tellurium slag, make it have stronger water-absorbent, tellurium mainly exists with water-soluble sodium tellurite form, all the other are the tellurite of water-fast sodium tellurate and heavy metal.The form that silicon in tellurium slag, selenium, arsenic, antimony, lead may exist is: Na
2siO
3, Na
2seO
3, Na
3asO
4, Na
3sbO
4, NaPbO
2; Copper and bismuth then exist in oxide form.
From tellurium slag, the method for separating tellurium mainly contains soda powder roasting method, alkaline high pressure lixiviation process, sulfurization roasting method, oxidation acid leaching method, extraction process, liquid-film method, microbial method, electrolytic refining process, vacuum distillation method, zone-melting and refining method etc. at present, be widely applied to industrial from tellurium slag, extract that tellurium adopts be water logging-electrodeposition process (Wang Liguo. bismuth is metallurgical. metallurgical industry press, 1986).This technique mainly comprises that ore grinding, water logging, purification, neutralization, roasting, alkali are molten, electrodeposition, multiple operation such as washing and founding, first first tellurium slag is crushed to 10 ~ 30mm, agitation leach after wet ball-milling again, leached mud returns the process of precious metals containing lead stove, leach liquor adds sodium sulphite and calcium chloride to remove the impurity such as lead, copper and silicon, and the solution sulfuric acid after purification is neutralized to pH=5 ~ 6 and obtains tellurium dioxide; Tellurium dioxide is dissolved in sodium hydroxide solution and carries out electrodeposition after roasting, negative electrode tellurium founding output tellurium ingot after the washing of rare oxalic acid solution.In addition, the tellurium slag of thick bismuth basic refining process output is also one of raw material reclaiming tellurium, and the production process extracting tellurium from this tellurium slag is similar to the technological process extracting tellurium from soda slag.
The leaching yield of tellurium slag conventional water leaching process tellurium only has about 70%, and still have the tellurium of considerable part to be present in conventional leached mud, it loses seriously when Returning smelting process, and this problem is the bottleneck that this technique of restriction is normally run.Because the leaching yield of traditional tellurium pulp water dipped journey tellurium is low, many people have studied the method (Liu Weifeng of acidic leaching, poplar natural feet, Ma Hui etc. a kind of method of separating tellurium from tellurium slag, ZL200910042937.4), but due to the change of solution system, there are two subject matters: one is that solution system is difficult to directly dock with meutral innersion, two is that in acid leaching solution, foreign matter content is higher, affects quality product.Patent application 201510204042.1 proposes the Strengthen education method of tellurium slag under existence condition while of adopting High Temperature High Pressure and additive, makes the MeTeO of indissoluble
3(Me is copper, lead and bismuth) is converted into Na
2teO
3dissolve, so improve the dipped journey of tellurium pulp water leaching yield (Liu Weifeng, Xiao Qingkai, Zhu Pengchun etc. a kind of method of tellurium slag Strengthen education, 201510204042.1).Although this Strengthen education method has increased substantially tellurium leaching yield, but deposit problem both ways, adopt High Temperature High Pressure means on the one hand, facility investment is large and running cost is high, undissolved tellurium is enriched in Strengthen education slag on the other hand, cause the content of tellurium in Strengthen education slag can up to 10-35%, so the recycling of this part tellurium be very valuable.
Summary of the invention is in order to overcome the deficiency of traditional tellurium slag Strengthen education Slag treatment method, the invention provides and a kind of adopt ball milling activation leaching method to realize tellurium in Strengthen education slag effectively to dissolve, and the Wet-process metallurgy method that tellurium leaching yield is high, simple to operate and processing cost is low.
In order to achieve the above object, the technical solution used in the present invention is: by tellurium slag Strengthen education slag according to joining in ball mill after certain liquid-solid ratio pulp, add sodium hydroxide and the sodium sulphite of requirement weight simultaneously, require to add abrading-ball according to control ratio of grinding media to material, then ball mill is started, certain hour is reacted under the ball milling system of regulation, undissolved tellurite or tellurate and sodium sulphite are reacted, the Na of generation
2teO
3dissolving enters solution, and heavy metal ion generates MeS precipitation and enters leached mud, and ball milling terminates rear mixed slurry and directly adopts vacuum filtration mode to realize solid-liquid separation, and tellurium ingot prepared traditionally by leach liquor, and leached mud reclaims other valuable metals again.The essence of the technical program is in alkaline sodium sulfide solution, utilize ball milling activation method that undissolved tellurite or tellurate are dissolved, and ball milling facilitates the carrying out of solubilizing reaction, improves the leaching yield of tellurium.
Concrete technological process and parameter as follows:
In alkaline sodium sulfide solution, adopt ball milling activation method to realize the abundant dissolving of tellurium slag Strengthen education slag.Strengthen education slag and water join pulp in the ball mill being with rubber liner by solid-to-liquid ratio (Strengthen education slag amount kg and liquor capacity L ratio) 1: 2.1 ~ 2.9, add the sodium hydroxide of Strengthen education slag weight 11.0 ~ 25.0% and the sodium sulphite of 16.0 ~ 30.0% simultaneously, then ball milling zirconia ball is added, control ratio of grinding media to material (zirconia ball weight Kg and Strengthen education slag weight Kg ratio) be 3 ~ 8: 1 and two kind of different diameter zirconia ball number ratio (diameter 10mm and diameter 5mm zirconia ball quantity ratio) be 1: 3, starting ball mill and keeping drum's speed of rotation to be 100-200r/min and slurry temperature is 50-95 DEG C, control turning direction regulation time and be spaced apart ball milling 4 ~ 6h under 0.5h condition, ball milling terminates rear mixed slurry and directly adopts vacuum filtration mode to realize solid-liquid separation, tellurium ingot prepared traditionally by leach liquor, leached mud reclaims other valuable metals again.The main chemical reactions that leaching process occurs is as follows:
(Me is Pb, Cu, Bi) (1)
ZrO in zirconia ball used
2mass percentage be greater than 95.0%.
The present invention is applicable to the Strengthen education slag processing anode sludge pyrometallurgical smelting process output tellurium slag, and its main component scope is (%) by weight percentage: Te15.0 ~ 35.0, Na5.0 ~ 10.0, Bi15.0 ~ 40.0, Ag1.5 ~ 15.0, Cu1.5 ~ 15.0 and Pb5.0 ~ 15.0.
The present invention and traditional tellurium slag leach and Strengthen education Measures compare, have following advantage: 1, the present invention with tellurium slag Strengthen education slag for raw material, in alkaline sodium sulfide solution, adopt ball milling activation method to make undissolved tellurite or tellurate continue to dissolve, have the advantage that tellurium leaching yield is high and simple to operate, when the activation of tellurium slag Strengthen education slag is leached, the leaching yield of tellurium can reach more than 75%; 2, the ball milling of traditional tellurium leaching process, leaching and purification three operations are incorporated in ball milling activation leaching process and carry out by the present invention, shorten technical process, achieve the depth extraction of tellurium in tellurium slag Strengthen education slag, reduce production cost, decrease material and overstock; What 3, the present invention obtained is low and do not affect follow-up tradition and extract the operating process of tellurium containing tellurium leach liquor foreign matter content; 4, the present invention has the advantage that technical process is short, technical indicator is stablized and labour intensity is low.
Accompanying drawing explanation
Fig. 1 is present invention process schematic flow sheet.
Embodiment
Embodiment 1:
Its main component of tellurium slag of anode sludge pyrometallurgical smelting process output is by weight percentage (%): Te29.97, Na13.54, Bi8.76, Ag0.68, Cu2.92 and Pb1.02, processing parameter during this slag Strengthen education: amount of sodium sulfide be tellurium slag weight 15%, liquid-solid ratio 3: 1, temperature 90 DEG C and time 2h, the leaching yield of tellurium can reach 95.42%, and in the Strengthen education slag of output, the mass percentage of tellurium is 22.37%.This tellurium slag Strengthen education slag adopts ball milling activation method to dissolve in alkaline sodium sulfide solution.Strengthen education slag and water join pulp in the ball mill being with rubber liner by solid-to-liquid ratio (Strengthen education slag amount kg and liquor capacity L ratio) 1: 2.5, add the sodium hydroxide of Strengthen education slag weight 15.0% and the sodium sulphite of 20.0% simultaneously, then add ball milling zirconia ball (wherein ZrO
2mass percentage be greater than 95.0%), control ratio of grinding media to material (zirconia ball weight Kg and Strengthen education slag weight Kg ratio) be 6: 1 and two kind of different diameter zirconia ball number ratio (diameter 10mm and diameter 5mm zirconia ball quantity ratio) be 1: 3, starting ball mill and keeping drum's speed of rotation to be 180r/min and slurry temperature is 75 DEG C, control turning direction regulation time and be spaced apart ball milling 5.0h under 0.5h condition, ball milling terminates rear mixed slurry and directly adopts vacuum filtration mode to realize solid-liquid separation, tellurium ingot prepared traditionally by leach liquor, leached mud reclaims other valuable metals again, when the activation of tellurium slag Strengthen education slag is leached, the leaching yield of tellurium is 76.32%.
Claims (2)
1. the method for a tellurium slag Strengthen education slag activation leaching, it is characterized in that comprising following process: Strengthen education slag and water join pulp in the ball mill of band rubber liner by solid-to-liquid ratio 1: 2.1 ~ 2.9, Strengthen education slag unit is kg, the volume of water is L, add the sodium hydroxide of Strengthen education slag weight 11.0 ~ 25.0% and the sodium sulphite of 16.0 ~ 30.0% respectively simultaneously, then ball milling zirconia ball is added, controlling ratio of grinding media to material is 3 ~ 8: 1, the zirconia ball number ratio of diameter to be 10mm and diameter be 5mm is 1: 3, starting ball mill and keeping drum's speed of rotation to be 100-200r/min and slurry temperature is 50-95 DEG C, the turning direction of a ball milling is adjusted every 0.5h, ball milling 4 ~ 6h, ball milling terminates rear mixed slurry and directly adopts vacuum filtration mode to realize solid-liquid separation, tellurium ingot prepared by leach liquor, leached mud reclaims other valuable metals again, described Strengthen education slag, be the Strengthen education slag of process anode sludge pyrometallurgical smelting process output tellurium slag, main component scope is by weight percentage: Te15.0 ~ 35.0, Na5.0 ~ 10.0, Bi15.0 ~ 40.0, Ag1.5 ~ 15.0, Cu1.5 ~ 15.0 and Pb5.0 ~ 15.0.
2. the method for tellurium slag Strengthen education slag activation leaching as claimed in claim 1, is characterized in that: ZrO in zirconia ball used
2mass percentage be greater than 95.0%.
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| CN201510984362.3A CN105506280A (en) | 2015-12-25 | 2015-12-25 | Activation leaching method of strengthened leaching tellurium residues |
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| CN201510984362.3A CN105506280A (en) | 2015-12-25 | 2015-12-25 | Activation leaching method of strengthened leaching tellurium residues |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106636661A (en) * | 2016-12-15 | 2017-05-10 | 中南大学 | Method for selectively separating and recovering tellurium and antimony from tellurium residues |
| CN111170277A (en) * | 2018-11-09 | 2020-05-19 | 中国瑞林工程技术股份有限公司 | Method for recovering bromine in electronic waste smelting smoke dust by wet alkaline system |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992280A (en) * | 2011-09-13 | 2013-03-27 | 郴州市金贵银业股份有限公司 | Technology for extracting tellurium dioxide from tellurium-containing smelting slag |
| JP2014189458A (en) * | 2013-03-27 | 2014-10-06 | Pan Pacific Copper Co Ltd | Tellurium recovery method |
| CN104445105A (en) * | 2014-11-24 | 2015-03-25 | 西北矿冶研究院 | Method for enriching and recovering tellurium dioxide from tellurium-containing soda residue |
-
2015
- 2015-12-25 CN CN201510984362.3A patent/CN105506280A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992280A (en) * | 2011-09-13 | 2013-03-27 | 郴州市金贵银业股份有限公司 | Technology for extracting tellurium dioxide from tellurium-containing smelting slag |
| JP2014189458A (en) * | 2013-03-27 | 2014-10-06 | Pan Pacific Copper Co Ltd | Tellurium recovery method |
| CN104445105A (en) * | 2014-11-24 | 2015-03-25 | 西北矿冶研究院 | Method for enriching and recovering tellurium dioxide from tellurium-containing soda residue |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106636661A (en) * | 2016-12-15 | 2017-05-10 | 中南大学 | Method for selectively separating and recovering tellurium and antimony from tellurium residues |
| 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 |
| CN111170277A (en) * | 2018-11-09 | 2020-05-19 | 中国瑞林工程技术股份有限公司 | Method for recovering bromine in electronic waste smelting smoke dust by wet alkaline system |
| CN111170277B (en) * | 2018-11-09 | 2023-03-10 | 中国瑞林工程技术股份有限公司 | Method for recovering bromine in electronic waste smelting smoke dust by wet alkaline system |
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Application publication date: 20160420 |