CN100463983C - Method for reclaiming metal by copper smelting-furnace magnesia brick lining - Google Patents
Method for reclaiming metal by copper smelting-furnace magnesia brick lining Download PDFInfo
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- CN100463983C CN100463983C CNB2007100120041A CN200710012004A CN100463983C CN 100463983 C CN100463983 C CN 100463983C CN B2007100120041 A CNB2007100120041 A CN B2007100120041A CN 200710012004 A CN200710012004 A CN 200710012004A CN 100463983 C CN100463983 C CN 100463983C
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Abstract
The present invention relates to metallurgical and chemical technology, and is especially process of recovering metals from magnesia brick as lining of copper smelting furnace. The process includes the following steps: crushing magnesia brick as the material, demagging, oxidizing roasting, extracting copper, deleading, and extracting gold and silver. The process can extract gold, silver, copper and other noble metals, recover magnesium sulfate and side products and protect environment.
Description
Technical field
What the present invention proposed is method metallurgical, that chemical field utilizes copper smelting-furnace magnesia brick lining recovery metal.
Background technology
The copper smelting is what to carry out under heating condition at the metallurgical furnace that is made of furnace lining magnesia brick, owing to except that containing copper, also contain precious metals such as gold and silver and lead in the copper ore concentrates, in the process of smelting, there is part metals to spread and absorbed by the magnesia fire-protecting wall of furnace lining.After the fire-resistant magnesia brick of furnace lining is damaged or reached work-ing life, promptly need to remove and change again and build furnace lining by laying bricks or stones.The magnesia fire-protecting wall of removing is dropped as waste material usually, and not only land occupation also can cause environmental pollution.Since in the magnesia fire-protecting wall of furnace lining adsorption and enrichment precious metals elements such as copper, lead, gold and silver, so be that raw material extracts the metallic element economically valuable and the value of environmental protection with copper smelting-furnace lining magnesia fire-protecting wall.
Summary of the invention
In order to extract metal from copper smelting-furnace lining magnesia fire-protecting wall, the present invention proposes a kind of method of utilizing copper smelting-furnace magnesia brick lining to reclaim metal.The mode that this method leaches by raw material roasting and step chemical solves the technical problem of metal recovery.
The present invention solves the scheme that its technical problem takes:
1, raw material pulverizing operation
To pulverize through the magnesia fire-protecting wall of the high metal content of hand picking to grind becomes powder, as the METAL EXTRACTION raw material.
2, de-magging operation
In the METAL EXTRACTION raw material, add sulfuric acid, make magnesium oxide transform into sal epsom, be dissolved in the sulphuric acid soln, the solid-state material of isolating as the roasting raw material.The solution crystallization that will contain sal epsom becomes solid magnesium sulfate.
3, oxidizing roasting operation
With the roasting of roasting raw material, make the part metals oxidation, be convenient to metallic element and leach.
4, extract copper process
Add sulfuric acid in the raw material after roasting, make copper change into copper sulfate and be dissolved in the aqueous solution, filtering separation, the solution that contains copper sulfate reclaims copper through the method for crystallization or electrodeposition, and isolated solid material slag carries out deleading to be handled.
5, deleading operation
Add sodium hydroxide or potassium hydroxide in the solid material slag after carrying copper, lead is wherein transformed in sodium plumbite or the water-soluble solution of potassium plumbite, leach the leaded aqueous solution, obtain containing gold and silver material slag, realized deleading.
6, extract gold and silver-colored operation
In the material slag that contains gold and silver, successively add nitric acid and nitric acid and vitriolic mixing acid, extract silver and golden respectively.
Can from the magnesia fire-protecting wall of copper smelting-furnace furnace lining, extract noble metals such as gold and silver and copper by method of the present invention; simultaneously all right reclaim(ed) sulfuric acid magnesium and lead, iron and chromium byproduct; from waste material, extract precious metals; the value of environmental protection that not only has environment protection also has the economic worth that turns waste into wealth.Be applicable to Industrial Metal smelting furnace body of heater lining to be that raw material extracts metal.
Description of drawings
Fig. 1 is a useful metal abstraction process procedure chart of the present invention
Among the figure, 1. raw material pulverizing operation, 2. de-magging operation, 3. oxidizing roasting operation is 4. extracted copper process, and 5. the deleading operation is 6. extracted gold and silver-colored operation.
Embodiment
With copper smelting-furnace furnace lining magnesia fire-protecting wall is raw material, carries out metal recovery according to operation process shown in Figure 1.
1, raw material pulverizing operation
To pulverize through the magnesia fire-protecting wall of the high metal content of hand picking to grind becomes powder, crosses 200 mesh sieves, as the METAL EXTRACTION raw material.
2, de-magging operation
A, in dilution heat of sulfuric acid, slowly add powdered roasting raw material, stir following and make it and react, reaction finishes the back dilute with water, extraction time is 1 hour for the first time, the supernatant liquor of above-mentioned leach liquor is inclined to, in extract, add dilute sulphuric acid, standing sedimentation then again, filtration washing forms the de-magging slag;
B, will through the supernatant liquor that leaching with in the light-magnesite powder and adjustment pH value be 6～7, with gained throw out filtering separation, the filtrate crystallisation by cooling is become the magnesium sulfate heptahydrate byproduct, isolated solid-state de-magging slag carries out calcination process.
3, oxidizing roasting operation
De-magging slag main component is chalcopyrite and alpha chalcocite, need to generate soluble metal vitriol, and iron rule changes into the ferric oxide of water insoluble and diluted acid through the copper in the sulphide ores being changed into the cupric oxide or the partial oxidation that are easily leached after the oxidizing roasting by sulfuric acid.With the roasting under 500～650 ℃ of temperature condition of de-magging slag, form fired slags, make the part metals oxidation, be convenient to leach.
4, extract copper process
Add sulfuric acid in the raw material after roasting, make copper change into copper sulfate and be dissolved in the aqueous solution, filtering separation, the solution that contains copper sulfate reclaims copper through the method for crystallization or electrodeposition, and isolated solid decopper(ing) slag carries out deleading to be handled.
Add aqueous sulfuric acid and leach copper, temperature in fired slags: 85～95 ℃, extraction time: 1～2 hour, reaction finished the back filtered while hot, and the filtrate of containing copper sulfate that obtains is told from solution through crystallization.Colourless with the hot wash filter residue until filtrate, collect and prepare dilution heat of sulfuric acid next time when filtrate is used for soaking copper.Obtain the decopper(ing) slag behind the filtration washing.
5, deleading operation
Add sodium hydroxide or potassium hydroxide aqueous solution in the decopper(ing) slag behind a, the Xiang Titong, lead is wherein transformed in sodium plumbite or the water-soluble solution of potassium plumbite, leach the leaded aqueous solution, obtain containing gold and silver material slag, realized deleading.
B, adding sulfuric acid in leaded filtrate, to adjust pH value be neutrality, and potassium plumbite or sodium plumbite change into lead sulfate, and precipitation is told.
(6), extract gold and silver-colored operation
A, desilver: add 15% nitric acid in containing gold and silver material slag, intermittent type stirs, and normal temperature leached 10 hours, add the entry dilution then, supernatant liquor is discharged in siphon after the sedimentation, filters, and wash leached mud with clear water, and in supernatant liquor and filtrate amalgamation liquid, add sodium-chlor, make silver change silver chloride into;
B, carry gold:, intermittently stir normal temperature leaching 10 hours to through adding nitric acid and vitriolic mixing acid (chloroazotic acid) in the material slag of desilver, in leaching vat, add the clear water dilution, filter, wash leached mud with water, filtrate is merged, adjust the pH value, obtain bronze with the S-WAT reduction to being 1～2.
Embodiment
3 tons on the useless magnesia brick of artificial picked at random copper smelting converter furnace lining.Levigate with the ball mill pulverizing to 200 orders, then with the sampling of division method.Chemical analysis data shows that the content of copper is 10.3% in the useless magnesia brick, and the content of silver is 898 μ gg
-1, the content of gold is 3 μ gg
-1From these experimental results, the metal in the useless magnesia brick has recovery value.Because content of magnesia is between 60%～65% in the useless magnesia brick, therefore reclaiming metal must remove magnesium oxide effectively, reclaims copper again after removing magnesium oxide, and silver-colored like this and gold can be highly enriched.
1, raw material pulverizing process:
To pulverize through the magnesia fire-protecting wall of the high metal content of hand picking to grind becomes powder, crosses 200 mesh sieves, as the METAL EXTRACTION raw material.
2, de-magging process:
By magnesian content in the useless magnesia brick is 60% calculating, and the useless magnesia brick of Theoretical Calculation per kilogram should consume 98%H
2SO
41.5kg, be actually and guarantee higher de-magging efficient, H
2SO
4Consumption should excessive 15%～20%.The mode that adopts substep to leach leaches, and reclaims by product sal epsom simultaneously.1.0kg H
2SO
4(560ml) be diluted to about 3L, slowly add the useless brick powder of 0.8kg, stir down, present the very exothermic reaction, reaction is diluted with water to 5L after finishing.Because very exothermic, do not seethe with excitement for making solution, must slowly add, the about 1h of extraction time for the first time inclines the supernatant liquor of above-mentioned leach liquor to go out, and remains about 2L, with 0.4kg H
2SO
4(220mL) be diluted to 1.5L, then with the 1.5L H for preparing
2SO
4Solution joins in the above-mentioned 2L extract, exothermic phenomenon still occurs, but and not serious, standing sedimentation then, filtration washing, 200g weighs after the drying.Slag rate 25%, leaching yield 75%, cupric 38.3% (weight percentage) in the de-magging slag, argentiferous 3127 μ gg-
2, contain golden 13.7 μ gg-
1The leaching yield in these data and the sulfuric acid de-magging process and the data of slag rate are consistent substantially, almost not loss of copper and silver in the de-magging process.The supernatant liquor that the first step is leached is with in the light-magnesite powder and to adjust the pH value be 6～7, at this moment Cr (OH)
3Be precipitated out the Fe (OH) of trace fully
3And Al (OH)
3Also be precipitated out fully.These throw outs are filtered out, at 60 ℃ of MgSO that adjust down after making with extra care
4The density of solution is 1.38g/mL, crystallisation by cooling, and obtaining purity is 98.5% magnesium sulfate heptahydrate byproduct, remaining Adlerika is back to use next time in the leach liquor.Secondary filtered liquid and washings are merged, be used for the dilute sulphuric acid of de-magging process preparation next time.
3, oxidizing roasting process:
De-magging slag main component is chalcopyrite (CuFeS
2), alpha chalcocite (Cu
9S
5), promptly use excessive sulfuric acid also can't leach copper, this also is the major cause that can successfully realize complete de-magging.The de-magging slag ingredient is complicated, the impurities element is more, need the copper in the sulphide ores to be changed into the cupric oxide that is easily leached by sulfuric acid through after the oxidizing roasting, therefore should carry out oxidizing roasting in advance before acidleach, roasting process depends on the completeness of maturing temperature and oxidation.Oxidizing roasting utilizes airborne oxygen and sulphide ores effect exactly, can generate oxide compound or vitriol by the different of temperature and gas phase composition.The former makes the metallic sulfide complete oxidation become oxide compound, also claims " dead roasting "; The latter then is that partial oxidation generates soluble metal vitriol, be called sulfurization roasting, and iron rule changes into the Fe of water insoluble and diluted acid
2O
3The de-magging slag is placed resistance furnace, and temperature is 500～650 ℃ in the control stove, is preferably in 550～600 ℃.In order to make the copper in the chalcopyrite be converted into cupric oxide fully, in roasting process, should frequently air door be opened, and constantly stir material, so that make the material of bottom have an opportunity fully to contact with air.Generally, breeze stirs once in 20～30min should be with stove.Material is not to there being blue look flame in the stove that detects by an unaided eye, and when not emitting Mars when stirring, illustrates that oxidizing roasting relatively fully.Roasting process is the process of weightening finish, and general per kilogram de-magging slag obtains 1.2～1.3kg fired slags after oxidizing roasting.In large-scale commercial production, can adopt boiling roaster, remove acid making system after the flue gas cooling.
4, extract the copper process:
Relatively the leaching condition of Shi Heing is: liquid-solid ratio (weight ratio) 4:1, fired slags and sulfuric acid weight ratio 1.1:1, extraction temperature: 85～95 ℃, extraction time: 1h adds 3.5kg water in the acid proof reaction flask, slowly adds 1.1kg 98% sulfuric acid then, after stirring, de-magging slag after the 1.26kg roasting is slowly added in the reactor, stirring reaction 1～2h, temperature of reaction is controlled at 85～95 ℃.Because of sour dissolution process is thermopositive reaction, and vitriolic dilution also has certain heat to emit, and therefore, initial reaction stage can rise to the temperature of requirement voluntarily, and the later stage needs heat tracing, and energy consumption is low.Reaction finishes the back filtered while hot, and the filtrate that obtains is sent the crystallizer crystallization, and is colourless until filtrate with the hot wash filter residue, preparation dilution heat of sulfuric acid when collection filtrate is used for soaking copper next time.Obtaining 0.26kg decopper(ing) slag behind the filtration washing, is 26% based on the slag rate of de-magging slag.Said process repeats ten times, collects the copper sulfate that obtains and obtains electro deposited copper 3.81kg through the method total of electrodeposition, and the direct yield that calculates copper is 99.5%.
5, deleading process:
Analytical results shows, lead content is 0.8% in the useless magnesia brick because de-magging and decopper(ing) all adopt sulfuric acid to leach, plumbously exist with the form of lead sulfate all the time because lead sulfate is water insoluble, thus lead sulfate by enrichment nearly 10 times.The method that adopts NaOH or KOH to leach is converted into Na with lead sulfate
2PbO
2Or K
2PbO
2And enter in the aqueous solution, separate after filtration, in filtrate, add H
2SO
4It is neutral adjusting the pH value, can obtain PbSO
4Precipitation.Precious metals such as gold and silver in the breeze after cleaning do not have any loss, have so just created favourable condition for metals such as subsequent recovery gold and silver.
6, extract silver and golden process:
A, desilver: through the above steps treating processes, gold and silver by enrichment nearly 20 times, handle that silver content has reached 1.6% in the slag, gold content has reached 68 μ gg
-1, adopting conventional leaching method is recyclable gold and silver.1.0kg material behind the above-mentioned deleading is added in the 5.0L large beaker, add 1.0L15% nitric acid, intermittent type stirs, and normal temperature leaches 10h, adds the dilution of 3.0L clear water in beaker, and supernatant liquor is discharged in siphon after the sedimentation.Filter, divide the washing leached mud four times, supernatant liquor and filtrate are merged, add 10g NaCl, obtain 11.40 silver chlorides with the 3.0L clear water.The nitric acid leached mud drying that filters out is weighed as 890g, and measuring wherein, the grade of silver is 58.8 μ gg
-1, the grade of lead slag-removed middle silver is 16000 μ gg
-1, the rate of recovery of silver is 99.7%.
B, carry gold: add 1L nitric acid and vitriolic mixing acid (chloroazotic acid) in above-mentioned 898g nitric acid leached mud, intermittent type stirs, and normal temperature leaches 10h, adds the 3L clear water and dilute in leaching vat.Filter, divide the washing leached mud four times with the 4L clear water, filtrate is merged, adjusting the pH value is 1～2, with the S-WAT reduction, obtains bronze 63mg.The grade of gold is 72 μ gg in the nitric acid leached mud
-1, the grade of gold is 1.8 μ gg in the chloroazotic acid leached mud
-1, the rate of recovery of gold is 96.8%.
(1), since in the sulfuric acid de-magging process by product sal epsom direct crystallization reclaim, so can reduce it, meet requirement on environmental protection to soil and contaminated water source, remaining Adlerika is back to use next time in the leach liquor after the crystallization, the Cr that filters out (OH)
3Can be used for producing the material of refractory brick Deng throw out, realize the effect of " zero release ".
(2), sulfur dioxide flue gas that roasting process produced can enter system for preparing sulfuric acid, or absorb, thereby eliminated atmospheric pollution by liming.
(3), the solution behind the electro deposited copper is ferrous through the condensing crystal reclaim(ed) sulfuric acid.
Claims (1)
1. utilize copper smelting-furnace magnesia brick lining to reclaim the method for metal, it is characterized in that: extract metal through raw material pulverizing operation (1), de-magging operation (2), oxidizing roasting operation (3), extraction copper process (4), deleading operation (5) and extraction gold and silver-colored operation (6), its procedure is:
(1), raw material pulverizing operation
To pulverize through the magnesia fire-protecting wall of the high metal content of hand picking to grind becomes powder, crosses 200 mesh sieves, as the METAL EXTRACTION raw material;
(2), de-magging operation
A, in dilution heat of sulfuric acid, slowly add powdered roasting raw material, stir following and make it and react, reaction finishes the back dilute with water, extraction time is 1 hour for the first time, the supernatant liquor of above-mentioned leach liquor is inclined to, in extract, add dilute sulphuric acid, standing sedimentation then again, filtration washing forms the de-magging slag;
B, will through the supernatant liquor that leaching with in the light-magnesite powder and adjustment pH value be 6～7, with gained throw out filtering separation, the filtrate crystallisation by cooling is become the magnesium sulfate heptahydrate byproduct, isolated solid-state de-magging slag carries out the oxidizing roasting operation;
(3), oxidizing roasting operation
With the roasting under 500～650 ℃ of temperature condition of roasting raw material, make the part metals oxidation, become fired slags;
(4), extract copper process
Add aqueous sulfuric acid in fired slags, temperature: 85～95 ℃, extraction time: 1～2 hour, reaction finished the back filtered while hot, obtained containing the filtrate of copper sulfate, and filtrate is told solid sulphuric acid copper through crystallization from solution, and the decopper(ing) slag that leaches enters the deleading operation;
(5), deleading operation
Add sodium hydroxide or potassium hydroxide aqueous solution in the decopper(ing) slag behind a, the Xiang Titong, lead is wherein transformed in sodium plumbite or the water-soluble solution of potassium plumbite, leach the leaded aqueous solution, obtain containing gold and silver material slag, realize deleading;
B, adding sulfuric acid in leaded filtrate, to adjust pH value be neutrality, and potassium plumbite or sodium plumbite change into lead sulfate, and precipitation is told;
(6), extract gold and silver-colored operation
A, desilver: add 15% nitric acid in containing gold and silver material slag, intermittent type stirs, and normal temperature leached 10 hours, add the entry dilution then, supernatant liquor is discharged in siphon after the sedimentation, filters, and wash leached mud with clear water, and in supernatant liquor and filtrate amalgamation liquid, add sodium-chlor, make silver change silver chloride into;
B, carry gold:, intermittently stir normal temperature leaching 10 hours to through adding nitric acid and vitriolic mixing acid in the material slag of desilver, in leaching vat, add the clear water dilution, filter, wash leached mud with water, filtrate is merged, and adjusting the pH value is 1～2, obtains bronze with the S-WAT reduction.
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| CN102382986A (en) * | 2011-10-20 | 2012-03-21 | 铜陵有色金属集团股份有限公司 | Treatment method of furnace bricks of Kaldo furnace |
| CN102925705A (en) * | 2012-11-28 | 2013-02-13 | 郴州市金贵银业股份有限公司 | Method for recovering valuable metals from furnace blocks of silver-refining furnaces |
| US20160319444A1 (en) | 2013-12-20 | 2016-11-03 | Greene Lyon Group, Inc. | Method and apparatus for recovery of noble metals, including recovery of noble metals from plated and/or filled scrap |
| CN110042241A (en) * | 2014-02-26 | 2019-07-23 | 格林里昂集团有限公司 | The recycling of gold and/or silver in waste material |
| WO2016210051A1 (en) | 2015-06-24 | 2016-12-29 | Greene Lyon Group, Inc. | Selective removal of noble metals using acidic fluids, including fluids containing nitrate ions |
| CN105385853B (en) * | 2015-11-12 | 2018-05-01 | 江西铜业技术研究院有限公司 | A kind of cupric gives up the processing method of magnesia brick |
| CN108823416B (en) * | 2018-07-06 | 2020-04-17 | 郴州市金贵银业股份有限公司 | Method for extracting gold and silver from clay graphite crucible slag |
| CN109055767A (en) * | 2018-10-23 | 2018-12-21 | 郴州市金贵银业股份有限公司 | A kind of method that gold and silver in clay-graphite crucible slag are extracted in alkali roasting |
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