CN103898332B - The technique that in copper scap metallurgical slag leaching process, copper zinc is separated with iron - Google Patents
The technique that in copper scap metallurgical slag leaching process, copper zinc is separated with iron Download PDFInfo
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- CN103898332B CN103898332B CN201210587187.0A CN201210587187A CN103898332B CN 103898332 B CN103898332 B CN 103898332B CN 201210587187 A CN201210587187 A CN 201210587187A CN 103898332 B CN103898332 B CN 103898332B
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Abstract
The present invention relates to 1, copper zinc is separated with iron in a kind of copper scap metallurgical slag leaching process technique, it comprises the following steps: (1) carries out Selectively leaching zinc to copper scap metallurgical slag; (2) selective leaching is slagged tap carry out weak-acid leaching; (3) solution after weak-acid leaching is heated and is added oxygenant, and copper zinc enters acid leaching solution, and iron enters acidic leaching residue; (4) copper extraction is carried out to acid leaching solution, realize being separated of copper and zinc-iron; (5) raffinate turns back in the step of Selectively leaching zinc, and zinc wherein enters selective leaching fluid and is recycled, and remaining copper iron enters into selective leaching through Selectively leaching process precipitation and slags tap.Present invention process has that flow process is short, investment and operation cost is low, simple to operate, leaching cycle is short, copper, zinc recovery advantages of higher, can realize the copper in environmental protection, efficient, Rapid Leaching copper scap metallurgical slag and zinc, and with iron separating metal copper.Be particularly suitable for processing the copper scap metallurgical slag that iron-holder is high, copper Zn content is high.
Description
Technical field
The present invention relates to the novel process that in a kind of copper scap metallurgical slag leaching process, copper zinc is separated with iron.
Background technology
In recent years, along with the demand of recycling economy and national environmental protection policy is strengthened, resource recovery comes into one's own day by day.A large amount of metallurgical slags can be produced as in the important component part copper scap cyclic regeneration process of copper resource recovery, these metallurgical slags now more adopts pyrogenic attack, along with the demand of national energy-saving environmental protection strengthens gradually, these metallurgical slags of wet processing become the trend of development.In the process of wet processing, certainly exist the problem of deironing, and the program being introduced separately into deironing will inevitably cause processing technological flow long, energy consumption is too high, therefore must explore new copper zinc and iron separating technology.
The method of the deironing that the main method that current copper zinc is separated with iron wet process is mainly traditional at present: goethite process, hematite process, ferrovanadium method, extraction process and neutralisation.These methods all need the step of independent deironing, increase the flow process of deironing, add the burden of large enterprises.When wet processing copper scap metallurgical slag, due to the specific properties of copper scap metallurgical slag, be main mainly with metal oxide in its slag, in treating processes, utilize this feature to be separated by part iron after leaching, by rational flow process, the concentration of iron in leaching process is controlled in rational scope.The content of iron can be controlled like this in leaching process, do not affect the leaching yield of copper zinc simultaneously, the object be separated of copper zinc and iron can be reached.
Summary of the invention
The object of this invention is to provide a kind of novel process making copper zinc be separated with iron in copper scap metallurgical slag leaching process.The conditions such as the joining day of this technology utilization reasonable manner and control temperature, extraction time and oxygenant realize the high efficiency separation of copper zinc and iron, reduction process copper scap metallurgical slag treatment scheme.
For achieving the above object, the present invention adopts following technical scheme:
1, the technique that in copper scap metallurgical slag leaching process, copper zinc is separated with iron, it is characterized in that, it comprises the following steps:
(1) carry out Selectively leaching to copper scap metallurgical slag, most of zinc enters in selective leaching fluid, and part zinc and copper iron enter during selective leaching slags tap;
(2) selective leaching is slagged tap carry out weak-acid leaching;
(3) solution after weak-acid leaching is heated and is added oxygenant, and copper zinc enters acid leaching solution, and iron enters acidic leaching residue;
(4) after copper zinc is separated with most of iron, copper extraction is carried out to acid leaching solution, realize being separated of copper and zinc-iron;
(5) raffinate turns back in the step of Selectively leaching zinc, and as Selectively leaching agent, zinc wherein enters selective leaching fluid and is recycled, and remaining copper iron enters into selective leaching through Selectively leaching process precipitation and slags tap.
Technique as above, preferably, before the Selectively leaching carrying out step (1), described copper scap metallurgical slag first divides through 60 mesh sieves, part large for granularity is separated, the little part of granularity is after magnetic separation Footwall drift iron, and gravity treatment Footwall drift copper, the copper scap metallurgical slag after magnetic separation and re-selection process is as leaching raw material.
Technique as above, preferably, described Selectively leaching and described weak-acid leaching leaching agent used are sulfuric acid, nitric acid or hydrochloric acid.
Technique as above, preferably, the concentration of described sulfuric acid is 40 ~ 200g/L.
Technique as above, preferably, the concentration of described nitric acid is 50 ~ 250g/L.
Technique as above, preferably, the concentration of described hydrochloric acid is 30 ~ 200g/L.
Technique as above, preferably, in the Selectively leaching process of step (1), control pH is 4.8 ~ 5.4, extraction time 0.5 ~ 1.5h, and extraction temperature is room temperature,
Technique as above, preferably, in the weak-acid leaching process of step (2), control pH is between 2.0 ~ 2.4, extraction time 1 ~ 1.5h, and extraction temperature is room temperature.
Technique as above, preferably, the control temperature of heating of step (3) is at 70 DEG C ~ 90 DEG C, and heating-up time 5min, adds oxygenant after intensification immediately, and described oxygenant is the H accounting for total amount of solution 2%
2o
2, and leaching raw material is evenly added in 30min, regulate pH between 5.0 ~ 5.4, leach when pH does not change in 5min and terminate.
Present invention process as above, in step (1), copper scap metallurgical slag is controlled extraction time by strict and leached acidity Selectively leaching zinc, the leaching yield of copper and iron is made to control below 0.1%, the leaching yield of zinc reaches about 60%, realize being separated of zinc and copper iron, selective leaching fluid, through the recyclable zinc of purification, does not need the step introducing deironing.In step (2) and (3), selective leaching is slagged tap through weak-acid leaching, and leach copper, zinc and iron wherein, now the leaching yield of copper zinc is more than 90%, the leaching yield of iron is about 60%, if now circulate by traditional mode, the accumulative speed of iron is very fast, and present invention process adds oxygenant after weak-acid leaching, and control other condition, can further improve the leaching yield of copper, zinc, can the most of iron in leach liquor is deposited in slag simultaneously, realize copper, zinc is separated with most of iron.In step (4), leach liquor is through copper extraction process, and reclaim the copper in leach liquor, remaining zinc and small part iron are in raffinate, and this part raffinate returns Selectively leaching operation as leaching agent.Selectively leaching operation can not only zinc in Selectively leaching raffinate in the step (5), the iron in raffinate can be sunk to during selective leaching is slagged tap simultaneously and go, in the turnover balance of the process implementation iron of circulation.
Beneficial effect of the present invention is:
The present invention proposes a kind of copper scap metallurgical slag New Process for Treatment of Treatment of Copper zinc-iron, according to the feature of copper scap metallurgical slag self, shorten the treatment scheme of process copper scap metallurgical slag, make full use of this secondary resource of copper scap metallurgical slag, improve comprehensive utilization of resources level, reduce environmental pollution, increase economic efficiency.The present invention is particularly suitable for each copper scap of China and smelts recovery factory, can adapt to the copper scap metallurgical slag processing various scale.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Specific implementation method
Below in conjunction with concrete embodiment, the invention will be further described, refers to Fig. 1, is the schema of copper scap metallurgical slag leaching process copper zinc of the present invention and iron separating technology.
(1) preliminary preparation is leached
Returned enterprise is smelted for the large-scale copper scap of China.This enterprise produces a large amount of copper scap metallurgical slags every year, and containing a large amount of copper zinc-irons in slag, its occurrence status is main mainly with oxide compound and metal alloy state.Copper scap metallurgical slag size-grade distribution is wide, must through screening.The boundary of screening is 60 orders, part large for grain is separated by screening, the little part of granularity after the metallic iron of magnetic separation recovery part, gravity treatment Footwall drift copper.Sample after magnetic separation and re-selection process operation is as leaching raw material, and wherein the content of each element is: copper 7.17%, zinc 30.43%, iron 3.82%.
(2) Selectively leaching process
Because copper scap metallurgical slag contains higher copper Zn content relative to ore smelting slag, the separation of copper, zinc can be realized when Selectively leaching in leaching process.Control extraction time 1h, leaching process strictly controls the pH fluctuation of leaching, pH controls 4.8 ~ 5.4, extraction temperature is room temperature, concentration of iron in leach liquor finally can be made at below 2mg/L, the concentration of copper is at 0.1g/L, and the leaching yield of zinc can close to 60%, and this part zinc solution just can produce zinc sulfate or electrowinning zinc through simple purification.At this moment selective leaching slag tap in containing most copper, iron and 40% zinc, will to its continue leach process.
(3) weak-acid leaching process
In order to leach remaining zinc and copper, and control the content of iron in leach liquor, weak-acid leaching will keep the pH of leaching process 2.0 ~ 2.4 all the time, extraction time 1.5h, extraction temperature is room temperature, when extraction time is reached home, the leaching yield of copper, zinc is more than 90%, the leaching yield of iron is about 60%, and the iron level in leach liquor is high, and can be more and more higher in the process of accumulation.When reaching leaching terminal, steam heats control temperature at about 80 DEG C, adds total amount of solution 2%H after intensification
2o
2, and slowly add leaching raw material, regulate pH between 5.0 ~ 5.2, this part-time is about 30min, and now the leaching yield of copper, zinc can more than 95%, and the iron after leaching can with Fe (OH)
3form come back in weak-acid leaching slag, thus realize being separated of copper zinc and iron, the total leaching yield of weak-acid leaching section of iron can drop to less than 30%.
(4) after passing through special efficacy copper extractant extracting copper after weak-acid leaching, in raffinate, the content of zinc and iron is constant, this part will return as Selectively leaching agent, leaching condition is controlled according to (2) again in the process of Selectively leaching, iron can enter into selective leaching and slag tap, and in working cycle, in leach liquor, the concentration of iron can not more than 10mg/L.
The trend leaching iron in flow process can be controlled by this circulation, if the inlet of iron is 3.82g in working cycle, the iron level of being walked out by the acidic leaching residue containing high ferro is about 3.80g, in working cycle, iron achieves balance, the separation of iron can be realized without independent iron removal step, reach cost-effective object.
Claims (6)
1. the technique that in copper scap metallurgical slag leaching process, copper zinc is separated with iron, it is characterized in that, it comprises the following steps:
(1) carry out Selectively leaching to the copper scap metallurgical slag after magnetic separation and re-selection process, most of zinc enters in selective leaching fluid, and part zinc and copper iron enter during selective leaching slags tap; In Selectively leaching process, control pH is 4.8 ~ 5.4, extraction time 0.5 ~ 1.5h, and extraction temperature is room temperature;
(2) slag tap to selective leaching and carry out weak-acid leaching, in weak-acid leaching process, control pH is between 2.0 ~ 2.4, extraction time 1 ~ 1.5h, and extraction temperature is room temperature;
(3) solution after weak-acid leaching is heated and is added oxygenant, and copper zinc enters acid leaching solution, and iron enters acidic leaching residue, wherein, control temperature of heating at 70 DEG C ~ 90 DEG C, heating-up time 5min, add oxygenant immediately after intensification, described oxygenant is the H accounting for total amount of solution 2%
2o
2, and leaching raw material is evenly added in 30min, regulate pH between 5.0 ~ 5.4, leach when pH does not change in 5min and terminate;
(4) after copper zinc is separated with most of iron, copper extraction is carried out to acid leaching solution, realize being separated of copper and zinc-iron;
(5) raffinate turns back in step (1), and as Selectively leaching agent, zinc wherein enters selective leaching fluid and is recycled, and remaining copper iron enters into selective leaching through Selectively leaching process precipitation and slags tap.
2. technique as claimed in claim 1, it is characterized in that, before the Selectively leaching carrying out step (1), described copper scap metallurgical slag first divides through 60 mesh sieves, part large for granularity is separated, the little part of granularity is after magnetic separation Footwall drift iron, and gravity treatment Footwall drift copper, the copper scap metallurgical slag after magnetic separation and re-selection process is as leaching raw material.
3. technique as claimed in claim 1 or 2, is characterized in that, described Selectively leaching and described weak-acid leaching leaching agent used are sulfuric acid, nitric acid or hydrochloric acid.
4. technique as claimed in claim 3, it is characterized in that, the concentration of described sulfuric acid is 40 ~ 200g/L.
5. technique as claimed in claim 3, it is characterized in that, the concentration of described nitric acid is 50 ~ 250g/L.
6. technique as claimed in claim 3, it is characterized in that, the concentration of described hydrochloric acid is 30 ~ 200g/L.
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| CN201210587187.0A CN103898332B (en) | 2012-12-28 | 2012-12-28 | The technique that in copper scap metallurgical slag leaching process, copper zinc is separated with iron |
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| CN105439357B (en) * | 2015-12-28 | 2018-11-20 | 中南大学 | Acid wastewater in mine recycling and deep-purifying method |
| CN110819816A (en) * | 2019-12-26 | 2020-02-21 | 中国葛洲坝集团绿园科技有限公司 | Method for recovering zinc from scrap copper smelting slag |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1900330A (en) * | 2006-06-30 | 2007-01-24 | 赤峰红烨锌冶炼有限责任公司 | Low pollution vanadium settling iron-removing wet zinc smelting method |
| CN101608258A (en) * | 2008-11-20 | 2009-12-23 | 厦门钨业股份有限公司 | Adopt cobalt-copper alloy to make the method that primary industry extracts cobalt, copper, iron |
| CN102560130A (en) * | 2010-12-15 | 2012-07-11 | 北京有色金属研究总院 | Selective leaching technology of copper and zinc in scrap copper smelting slag |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1900330A (en) * | 2006-06-30 | 2007-01-24 | 赤峰红烨锌冶炼有限责任公司 | Low pollution vanadium settling iron-removing wet zinc smelting method |
| CN101608258A (en) * | 2008-11-20 | 2009-12-23 | 厦门钨业股份有限公司 | Adopt cobalt-copper alloy to make the method that primary industry extracts cobalt, copper, iron |
| CN102560130A (en) * | 2010-12-15 | 2012-07-11 | 北京有色金属研究总院 | Selective leaching technology of copper and zinc in scrap copper smelting slag |
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