CN107604171A - A kind of method of the melting enriching noble metals from complicated high content of nickel copper anode mud leached mud - Google Patents
A kind of method of the melting enriching noble metals from complicated high content of nickel copper anode mud leached mud Download PDFInfo
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Abstract
The invention discloses a kind of method of the melting enriching noble metals from complicated high content of nickel copper anode mud leached mud, raw material, flux, cosolvent, reducing agent are sufficiently mixed by this method, pretreatment of raw material pelletizing method is carried out to make from fluxed sintering feed, then melting is carried out, the noble metals such as Gold, Silver, Platinum, Palladium selen-tellurjum are made to fully enter precious metals containing lead alloy melt, the selective reduction of other impurities element enters precious metals containing lead alloy melt, remaining largely enters in smelting slag melt, and wherein silicon, barium compound are fully entered in smelting slag melt.The physical sensible heat of the process makes full use precious metals containing lead alloy melt and smelting slag melt, the step of process melt and slag heat energy comprehensive utilization up and down is realized, cold burden heating times is reduced, reaches energy-saving purpose；The noble metal rate of recovery is high, and while enriching noble metals are realized, lead bismuth valuable metal can comprehensively utilize；In addition, present invention process is simple, environment-friendly, easy to operate, labor intensity is small, efficiency high, and production process is easily controlled.
Description
Technical field
The invention belongs to rare precious metal pyro-refining-vacuum fusion separated technical field, and in particular to a kind of from multiple
The method of melting enriching noble metals in miscellaneous high content of nickel copper anode mud leached mud.
Background technology
Copper anode mud pressure leaching slag uses Kaldo Furnace melting converting process, by process optimization in recent years, skill
Art is transformed and the horizontal lifting of operational administrative, the technical-economic index of production steadily improve.But, however it remains your dilute gold such as gold and silver
Belong to the problems such as direct yield is relatively low, flux cost is high.
The production of copper anode mud pressure leaching slag concentration smelting typically uses Na2O-SiO2System, the actual system is PbO-
Na2O-BaO-SiO2System, copper anode mud pressure leaching slag Kaldo Furnace melting blowing add coke as reducing agent, sodium carbonate,
Quartz is as fluxing agent slag making.Due to Na2CO3Price, cost are high, belong to strong basicity flux, and substantial amounts of sodium oxide molybdena gasification is waved
Hair loss is serious, and efficiency is low, pollution environment, and the sodium oxide molybdena erosion of refractory of decomposition, lining durability is short, repaiies stove cost
Height, reduce Kaldo Furnace operating rate.In addition, the slag mobility formed is strong, difficulty of skimming.
Due to deficiency more than existing, in order to realize efficiently separating for precious metals containing lead alloy and gangue, make gangue and ash content in slag making
During be melted into the clinker of liquid, and there is good mobility, clinker should have suitable chemical composition, good thing
Rationality matter, good technical-economic index can be obtained, meanwhile, be advantageous to protect furnace lining, extending furnace lining life.Precious metals containing lead alloy melts
The chemical composition and physical property of furnace slag, precious metals containing lead alloy metallurgy process and technical-economic index are influenceed very big.Precious metals containing lead is smelted
Slag making is with basic solvent and acidic flux and the acid in the alkaline matter and acidic materials and reducing agent and fuel in material
Property ash content chemically react, the small clinker of generation low melting point, density, and by the material dissolving insoluble in precious metals containing lead alloy melt,
Converge the process of slagging.
Copper anode mud pressurization slag ingredient (unit Pt, Pd g/t；Remaining %)：Ni3.6、Cu4.2、Pb21.73、Bi2.69、
Sb3.60、As0.59、SiO23.51、Au0.2719、Ag3.56、Pt139、Pd236、Se3.78。
The content of the invention
The invention aims to solve technical problem present in prior art, there is provided a kind of technique is simple, environment
Friendly, easy to operate, energy-saving, production process is easily controlled, the noble metal rate of recovery is high and is realizing the same of enriching noble metals
When, the method for melting enriching noble metals from complicated high content of nickel copper anode mud leached mud that lead bismuth valuable metal can comprehensively utilize.
In order to achieve the above object, the present invention uses following technical scheme：It is a kind of from complicated high content of nickel copper anode mud leached mud
The method of middle melting enriching noble metals, this method comprise the following steps：
Step 1, high content of nickel copper anode mud leached mud, flux, fluxing agent, reducing agent be sufficiently mixed uniformly, by compound in disk
On pelletizer plus water soaks pelletizing, forms a diameter of 5-8mm pelletizing；
Step 2, pelletizing is put into rotary kiln the baking and concretion under conditions of 350-400 DEG C of temperature formed it is spherical from fluxed burning
Ramming material, natural cooling after roasting；
Step 3, it will be melted in the spherical addition intermediate frequency furnace cinder ladle from fluxed sintering feed after cooling, it is 1350 to control smelting temperature
DEG C, soaking time 30min；
Step 4, reaction finish furnace temperature and are down to 800-850 DEG C of separation precious metals containing lead alloy melt and smelting slag melt, smelting slag after separation
Melt and precious metals containing lead alloy melt difference hot-loading and hot-conveying；
Step 5, add precious metals containing lead alloy melt quality 0.3-0.5%'s in precious metals containing lead alloy melt when temperature is down to 400-450 DEG C
Wood sawdust, precious metals containing lead alloy melt quality 1-2% coke blacking, precious metals containing lead alloy melt quality 1-2% sodium carbonate liquate remove ambrose alloy, melt
It is stirred continuously in analysis course of reaction, drags for slag, the liquate reaction time is 1-3h；
Oxidation blowing is carried out to precious metals containing lead alloy melt after step 6, liquate, obtains electrum melt and blowing slag melt；
Step 7, slag melt hot-loading and hot-conveying to the reduction furnace that will blow carry out injection melting and reducing and obtain the thick alloy melt of lead bismuth and melt
Refine slag melt；
Step 8, smelting slag melt hot-loading and hot-conveying in step 4 to reduction furnace is carried out being blown melting and reducing obtain the thick alloy of lead bismuth and melt
Body and reducing slag；
Step 9, the thick alloy melt hot-loading and hot-conveying of lead bismuth that step 7 and step 8 obtain steamed to vacuum metallurgy furnace through vacuum fusion
Cut is from obtaining the dilute noble alloy of vacuum drying oven and lead bismuth alloy.
Further, flux is lime and quartz in the step 1, and fluxing agent is sodium carbonate, and reducing agent is coke blacking.
Further, in the step 1 lime adding amount be high content of nickel copper anode mud leached mud quality 0.5-2.5%, carbonic acid
Sodium addition is the 1-2% of high content of nickel copper anode mud leached mud quality, and coke blacking addition is high content of nickel copper anode mud leached mud quality
1%, quartzy addition is the 1% of high content of nickel copper anode mud leached mud quality.
Further, amount of water is the 15-25% of high content of nickel copper anode mud leached mud quality during pelletizing in the step 1.
Further, the granularity of the coke blacking is less than or equal to 200 mesh.
Further, in the step 7 and step 8 be blown melting and reducing temperature be 1300 DEG C, time 40min.
Further, the vacuum in the step 9 during vacuum metallurgy furnace vacuum metallurgy be 3-18Pa, temperature 1000-
1050 DEG C, time 2.0h.
The present invention has the advantages that compared with the prior art：The present invention is using " fiery a melting-vacuum fusion distillation point
From " technical matters, by complicated high content of nickel copper anode mud leached mud after melting, reducing, smelting slag and blowing slag hot-loading and hot-conveying, respectively
Be blown the process of Reducing Lead bismuth and rare precious metal.To obtain the preferable slag type of low melting point, using CaO-SiO2System flux,
Appropriate quartz and lime are first added in complicated high content of nickel copper anode mud leached mud as flux, adds appropriate sodium carbonate conduct
Fluxing agent, appropriate coke blacking is added as reducing agent, raw material, flux, cosolvent, reducing agent are sufficiently mixed, carry out raw material
Pretreatment-pelletizing method is made from fluxed sintering feed, is then carried out melting, is fully entered the noble metals such as Gold, Silver, Platinum, Palladium selen-tellurjum expensive
Metal melt, the selective reduction of other impurities element enter precious metals containing lead alloy melt, and remaining largely enters in smelting slag melt,
Wherein silicon, barium compound are fully entered in smelting slag melt.The process makes full use precious metals containing lead alloy melt and smelting slag melt
Physical sensible heat, the step of process melt and slag heat energy comprehensive utilization up and down is realized, reduces cold burden heating times, reaches energy-conservation drop
The purpose of consumption；The noble metal rate of recovery is high, and while enriching noble metals are realized, lead bismuth valuable metal can comprehensively utilize；In addition, this
Invented technology is simple, environment-friendly, does not produce poisonous waste gas and waste residue etc., also without using poisonous reagent, meets environment
The requirement of protection；And it is easy to operate, labor intensity is small, efficiency high, and production process is easily controlled, and is also easy to the automatic of implementation process
Change.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of method of the melting enriching noble metals from complicated high content of nickel copper anode mud leached mud comprises the following steps：
Step 1, high content of nickel copper anode mud leached mud 150kg, flux, fluxing agent, reducing agent be sufficiently mixed uniformly, flux is lime
And quartz, fluxing agent are sodium carbonate, reducing agent is the coke blacking that granularity is less than or equal to 200 mesh, and lime adding amount is high ambrose alloy sun
The 0.5% of pole mud leached mud quality（0.75 kg）, sodium carbonate addition is the 2% of high content of nickel copper anode mud leached mud quality（3 kg）,
Coke blacking addition is the 1% of high content of nickel copper anode mud leached mud quality（1.5 kg）, quartzy addition is the leaching of high content of nickel copper anode mud
The 1% of slag amount（1.5 kg）, compound is added to water wetting pelletizing on disc balling machine, amount of water is that high content of nickel copper anode mud soaks
The 15% of quality of slagging tap（22.5 kg）, a diameter of 5-8mm pelletizing is formed after pelletizing.
Step 2, pelletizing is put into rotary kiln the baking and concretion under conditions of 350 DEG C of temperature formed it is spherical from fluxed burning
Ramming material, natural cooling after roasting.
Step 3, spherical added from fluxed sintering feed in intermediate frequency furnace cinder ladle that will be after cooling are melted, and control the smelting temperature to be
1350 DEG C, soaking time 30min.
Step 4, reaction finish furnace temperature and are down to 850 DEG C of separation precious metals containing lead alloy melts and smelting slag melt, smelting slag after separation
Melt and precious metals containing lead alloy melt difference hot-loading and hot-conveying.Smelting slag melt chemistry composition（%, Au, Pt, Pd unit are (g/t)）For：
Ag1.15、Au144、Pt7.67、Pd10.5、Ni3.18、Cu0.22、Pb28.08、Bi0.29、As1.12、Sb7.16、Se0.12、
Te0.029、CaO0.12、SiO213.69。
Step 5, the sawmilling that precious metals containing lead alloy melt quality 0.3% is added when temperature is down to 400 DEG C in precious metals containing lead alloy melt
Bits, the sodium carbonate liquate of the coke blacking of precious metals containing lead alloy melt quality 2%, precious metals containing lead alloy melt quality 1% remove ambrose alloy, and liquate reacted
It is stirred continuously in journey, drags for slag, the liquate reaction time is 3h.
Oxidation blowing is carried out to precious metals containing lead alloy melt after step 6, liquate, obtains electrum melt and blowing slag melt.
Step 7, slag melt hot-loading and hot-conveying to the reduction furnace that will blow carry out injection melting and reducing and obtain the thick alloy melt of lead bismuth
With smelting slag melt, injection melting and reducing temperature is 1300 DEG C, time 40min.
Step 8, smelting slag melt hot-loading and hot-conveying in step 4 to reduction furnace is carried out being blown melting and reducing obtain lead bismuth and slightly close
Golden melt and reducing slag, injection melting and reducing temperature is 1300 DEG C, time 40min.
Step 9, the thick alloy melt hot-loading and hot-conveying of lead bismuth that step 7 and step 8 obtain melted to vacuum metallurgy furnace through vacuum
Melt separated, vacuum during vacuum metallurgy furnace vacuum metallurgy is 18Pa, temperature is 1000 DEG C, time 2.0h, and vacuum melts
Melt separated and obtain the dilute noble alloy of vacuum drying oven and lead bismuth alloy.The dilute noble alloy composition of vacuum drying oven（Pt, Pd, Au unit g/t, its
Remaining element is %）For：Ag15.3、Pt5002、Pd1600、Au1300、Ni11.96、Cu7.51、Pb0.26、As1.02、
Sb37.15、Bi0.057；Lead bismuth alloy composition（Pt, Pd, Au unit g/t, remaining element are %）For：Ag0.14、Pt34.3、
Pd9.56、Au7.76、Ni0.021、Cu0.037、Pb89.72、As0.23、Sb25.12、Bi5.58。
Embodiment 2
A kind of method of the melting enriching noble metals from complicated high content of nickel copper anode mud leached mud comprises the following steps：
Step 1, high content of nickel copper anode mud leached mud 150kg, flux, fluxing agent, reducing agent be sufficiently mixed uniformly, flux is lime
And quartz, fluxing agent are sodium carbonate, reducing agent is the coke blacking that granularity is less than or equal to 200 mesh, and lime adding amount is high ambrose alloy sun
The 2.5% of pole mud leached mud quality（3.75 kg）, sodium carbonate addition is the 1% of high content of nickel copper anode mud leached mud quality（1.5
kg）, coke blacking addition is the 1% of high content of nickel copper anode mud leached mud quality（1.5 kg）, quartzy addition is high content of nickel copper anode mud
The 1% of leached mud quality（1.5 kg）, compound is added to water wetting pelletizing on disc balling machine, amount of water is high content of nickel copper anode
The 25% of mud leached mud quality（37.5 kg）, a diameter of 5-8mm pelletizing is formed after pelletizing.
Step 2, pelletizing is put into rotary kiln the baking and concretion under conditions of 400 DEG C of temperature formed it is spherical from fluxed burning
Ramming material, natural cooling after roasting.
Step 3, spherical added from fluxed sintering feed in intermediate frequency furnace cinder ladle that will be after cooling are melted, and control the smelting temperature to be
1350 DEG C, soaking time 30min.
Step 4, reaction finish furnace temperature and are down to 800 DEG C of separation precious metals containing lead alloy melts and smelting slag melt, smelting slag after separation
Melt and precious metals containing lead alloy melt difference hot-loading and hot-conveying.Smelting slag melt chemistry composition（%, Au, Pt, Pd unit are (g/t)）For：
Ag52.92、Au1.30、Pt623、Pd1000、Ni1.24、Cu2.18、Pb6.14、Bi0.065、As0.93、Sb6.51、
Se14.48、Te3.87、CaO4.30、SiO219.51。
Step 5, the sawmilling that precious metals containing lead alloy melt quality 0.5% is added when temperature is down to 450 DEG C in precious metals containing lead alloy melt
Bits, the sodium carbonate liquate of the coke blacking of precious metals containing lead alloy melt quality 1%, precious metals containing lead alloy melt quality 2% remove ambrose alloy, and liquate reacted
It is stirred continuously in journey, drags for slag, the liquate reaction time is 1h.
Oxidation blowing is carried out to precious metals containing lead alloy melt after step 6, liquate, obtains electrum melt and blowing slag melt.
Step 7, slag melt hot-loading and hot-conveying to the reduction furnace that will blow carry out injection melting and reducing and obtain the thick alloy melt of lead bismuth
With smelting slag melt, injection melting and reducing temperature is 1300 DEG C, time 40min.
Step 8, smelting slag melt hot-loading and hot-conveying in step 4 to reduction furnace is carried out being blown melting and reducing obtain lead bismuth and slightly close
Golden melt and reducing slag, injection melting and reducing temperature is 1300 DEG C, time 40min.
Step 9, the thick alloy melt hot-loading and hot-conveying of lead bismuth that step 7 and step 8 obtain melted to vacuum metallurgy furnace through vacuum
Melt separated, vacuum during vacuum metallurgy furnace vacuum metallurgy is 3Pa, temperature is 1050 DEG C, time 2.0h, vacuum fusion
Separated obtains the dilute noble alloy of vacuum drying oven and lead bismuth alloy.The dilute noble alloy composition of vacuum drying oven（Pt, Pd, Au unit g/t, remaining
Element is %）For：Ag13.20、Pt5420、Pd1610、Au1330、Ni13.31、Cu8.16、Pb0.14、As1.52、Sb33.18、
Bi0.0062；Lead bismuth alloy composition（Pt, Pd, Au unit g/t, remaining element are %）For：Ag0.16、Pt13.7、Pd17.0、
Au14.0、Ni0.023、Cu0.070、Pb79.44、As0.34、Sb12.28、Bi6.67。
Claims (7)
- A kind of 1. method of the melting enriching noble metals from complicated high content of nickel copper anode mud leached mud, it is characterised in that this method includes Following steps：Step 1, high content of nickel copper anode mud leached mud, flux, fluxing agent, reducing agent be sufficiently mixed uniformly, by compound in disk On pelletizer plus water soaks pelletizing, forms a diameter of 5-8mm pelletizing；Step 2, pelletizing is put into rotary kiln the baking and concretion under conditions of 350-400 DEG C of temperature formed it is spherical from fluxed burning Ramming material, natural cooling after roasting；Step 3, it will be melted in the spherical addition intermediate frequency furnace cinder ladle from fluxed sintering feed after cooling, it is 1350 to control smelting temperature DEG C, soaking time 30min；Step 4, reaction finish furnace temperature and are down to 800-850 DEG C of separation precious metals containing lead alloy melt and smelting slag melt, smelting slag after separation Melt and precious metals containing lead alloy melt difference hot-loading and hot-conveying；Step 5, add precious metals containing lead alloy melt quality 0.3-0.5%'s in precious metals containing lead alloy melt when temperature is down to 400-450 DEG C Wood sawdust, precious metals containing lead alloy melt quality 1-2% coke blacking, precious metals containing lead alloy melt quality 1-2% sodium carbonate liquate remove ambrose alloy, melt It is stirred continuously in analysis course of reaction, drags for slag, the liquate reaction time is 1-3h；Oxidation blowing is carried out to precious metals containing lead alloy melt after step 6, liquate, obtains electrum melt and blowing slag melt；Step 7, slag melt hot-loading and hot-conveying to the reduction furnace that will blow carry out injection melting and reducing and obtain the thick alloy melt of lead bismuth and melt Refine slag melt；Step 8, smelting slag melt hot-loading and hot-conveying in step 4 to reduction furnace is carried out being blown melting and reducing obtain the thick alloy of lead bismuth and melt Body and reducing slag；Step 9, the thick alloy melt hot-loading and hot-conveying of lead bismuth that step 7 and step 8 obtain steamed to vacuum metallurgy furnace through vacuum fusion Cut is from obtaining the dilute noble alloy of vacuum drying oven and lead bismuth alloy.
- 2. a kind of method of melting enriching noble metals from complicated high content of nickel copper anode mud leached mud according to claim 1, It is characterized in that：Flux is lime and quartz in the step 1, and fluxing agent is sodium carbonate, and reducing agent is coke blacking.
- 3. a kind of method of melting enriching noble metals from complicated high content of nickel copper anode mud leached mud according to claim 2, It is characterized in that：Lime adding amount is the 0.5-2.5% of high content of nickel copper anode mud leached mud quality in the step 1, and sodium carbonate adds It is the 1% of high content of nickel copper anode mud leached mud quality to measure as the 1-2% of high content of nickel copper anode mud leached mud quality, coke blacking addition, stone English addition is the 1% of high content of nickel copper anode mud leached mud quality.
- 4. a kind of method of melting enriching noble metals from complicated high content of nickel copper anode mud leached mud according to claim 1, It is characterized in that：Amount of water is the 15-25% of high content of nickel copper anode mud leached mud quality during pelletizing in the step 1.
- 5. a kind of method of melting enriching noble metals from complicated high content of nickel copper anode mud leached mud according to claim 2, It is characterized in that：The granularity of the coke blacking is less than or equal to 200 mesh.
- 6. a kind of method of melting enriching noble metals from complicated high content of nickel copper anode mud leached mud according to claim 1, It is characterized in that：In the step 7 and step 8 be blown melting and reducing temperature be 1300 DEG C, time 40min.
- 7. a kind of method of melting enriching noble metals from complicated high content of nickel copper anode mud leached mud according to claim 1, It is characterized in that：Vacuum in the step 9 during vacuum metallurgy furnace vacuum metallurgy is 3-18Pa, temperature is 1000-1050 DEG C, Time is 2.0h.
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| CN108456778A (en) * | 2018-03-27 | 2018-08-28 | 广州万仕智投资有限公司 | A method of electrum is produced by rich and honour lead |
| CN109536712A (en) * | 2018-11-14 | 2019-03-29 | 昆明理工大学 | A method of it being simple and efficient recycling copper and tellurium from copper tellurium slag |
| CN110699541A (en) * | 2019-10-23 | 2020-01-17 | 金川集团股份有限公司 | Process for treating complex tailings by using rotary kiln |
| CN110760688A (en) * | 2019-10-23 | 2020-02-07 | 金川集团股份有限公司 | Method for deeply removing impurities and enriching precious metals in complex lead-bismuth alloy |
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