CN104946883B - A kind of preprocess method of copper anode mud - Google Patents
A kind of preprocess method of copper anode mud Download PDFInfo
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Abstract
The invention provides a kind of preprocess method of copper anode mud, it comprises the following steps：Copper anode mud is filtered successively, dry and ball-milling treatment；Copper anode mud is added to progress pyrogenic process chlorination in rotary kiln or fluidized roaster；Alkaline leaching processing is carried out to copper anode mud, obtains alkaline leaching liquid and alkaline leaching slag；Acidic leaching processing is carried out to alkaline leaching slag, obtains the acidic leaching residue of acid leaching solution and enriching noble metals, pretreatment operation is completed.The preprocess method of copper anode mud provided by the invention, it carries out pyrogenic process chlorination by using rotary kiln or fluidized roaster to copper anode mud, so that selenium, tellurium chloride-sublimation after chlorination and enter flue gas, separated with chloride slag, the removing of selenium and tellurium is complete, solve the scattering problem of selenium and tellurium in whole copper anode slime treatment process, reduce and even avoid the influence of selenium, tellurium metal to gold and silver product quality, and such a mode of operation also allows for the centralized recovery of selenium and tellurium.
Description
Technical field
The present invention relates to metallurgical technology field, more specifically to a kind of preprocess method of copper anode mud.
Background technology
At present, the primary raw material of copper metallurgy is copper-sulphide ores in the world, but makees raw material using such a copper-sulphide ores, with wet method
It is higher to extract the cost of copper, therefore, various countries are more based on copper smelting by pyrometallurgy, and the yield of copper smelting by pyrometallurgy accounts for the 80% of world's copper yield.
During copper smelting by pyrometallurgy, copper anode mud is the insoluble matter that anode copper obtains in electrorefining, copper anode mud
In contain substantial amounts of valuable metal, be the important source material for extracting the noble metal such as Au Ag Pt Pd, its yield is generally cathode copper production
The 0.2%~0.8% of amount, reaches as high as 1.4%.As enterprise's copper anode mud treating capacity increasingly increases, how more efficient processing has
The copper anode mud of higher-value allows for allowing people more to pay close attention to.
Valuable metal exists in the form of simple substance, oxide and complex compound etc. in copper anode mud, in order to extract copper anode
Noble metal in mud, need first to be separated and recovered from other base metals in copper anode mud, i.e., to copper anode before noble metal is extracted
Mud is pre-processed, and remove influences the foreign metals such as big copper, arsenic, selenium, tellurium to noble metal extraction process.In the prior art,
Numerous studies work has been done in pretreatment of the expert and research personage of nonferrous smelting industry for copper anode mud, develops air oxygen
Change decopper(ing) method, oxidizing roasting method, sulfating roasting method, soda roasting method, sulfuric acid system pressure oxidation leaching-out method, beneficiation enrichment method
Etc. a variety of methods.Although these copper anode mud preprocess methods respectively have advantage, inventor has found that they all have identical
The separating effect of selenium, tellurium metal in shortcoming, i.e. copper anode mud is undesirable, and in whole preprocessing process, selenium, tellurium metal are all the time
It is scattered in copper anode mud, has had a strong impact on that the gold and silver product subsequently obtained is quality.
Therefore, the influence of selenium, tellurium metal to gold and silver product quality how is reduced or even avoided, is current people in the art
Member's urgent problem to be solved.
The content of the invention
In view of this, the invention provides a kind of preprocess method of copper anode mud, it fully and can concentrate selenium, tellurium
Separation, reduce even avoid the influence of selenium, tellurium metal to gold and silver product quality.
In order to achieve the above object, the present invention provides following technical scheme：
A kind of preprocess method of copper anode mud, it comprises the following steps：
1）The copper anode mud is filtered successively, dry and ball-milling treatment；
2）Then the copper anode mud is added to progress pyrogenic process chlorination in rotary kiln or fluidized roaster, will reaction
Obtained selenium and the chloride of tellurium is separated in the form of flue dust with the copper anode mud；
3）Alkaline leaching processing is carried out to the copper anode mud again, obtains alkaline leaching liquid and alkaline leaching slag；
4）Acidic leaching processing finally is carried out to the alkaline leaching slag, obtains the acid of acid leaching solution and enriching noble metals
Property leached mud.
Preferably, in the preprocess method of above-mentioned copper anode mud, when processing is dried to the copper anode mud, drying temperature
Spend for 100 DEG C~105 DEG C, and 2~3 hours are incubated to the copper anode mud.
Preferably, in the preprocess method of above-mentioned copper anode mud, when carrying out ball-milling treatment to the copper anode mud, during ball milling
Between be 1 hour~3 hours.
Preferably, in the preprocess method of above-mentioned copper anode mud, when carrying out pyrogenic process chlorination, the rotary kiln or fluidization
Temperature in roaster is 300 DEG C~500 DEG C.
Preferably, in the preprocess method of above-mentioned copper anode mud, when carrying out alkaline leaching processing, the copper after chlorination
The earth of positive pole is 1molL with concentration in retort-1~3molL-1Sodium hydroxide solution pulp, liquid-solid ratio 4:1~8:
1, in temperature 70 C~90 DEG C, leach 2 hours~5 hours；Cooled after reaching the reaction time, when temperature be reduced to 65 DEG C with
Under, slurry and separation of solid and liquid are released, obtains alkaline leaching liquid and alkaline leaching slag.
Preferably, in the preprocess method of above-mentioned copper anode mud, when carrying out acidic leaching processing, the alkaline leaching slag
With concentration it is 1.5molL in retort-1~4molL-1Sulfuric acid solution pulp, liquid-solid ratio 4:1~8:1, in temperature
70 DEG C~90 DEG C, leach 2 hours~5 hours；Reach and slurry and separation of solid and liquid released after the reaction time, obtain acid leaching solution and
The acidic leaching residue of enriching noble metals.
In the preprocess method of copper anode mud provided by the invention, segment processing is carried out to copper anode mud, first to copper anode
Mud is filtered, dry and ball milling, then carries out pyrogenic process chlorination, chlorination to copper anode mud using rotary kiln or fluidized roaster
Selenium, the tellurium chloride obtained afterwards evaporates into flue dust state in rotary kiln or fluidized roaster and entered in flue gas, so as to
Realize the copper anode mud with solid-state（Copper anode mud now is referred to as chloride slag）It is abundant, concentrate separation, chloride slag is again
Handled by alkaline leaching, the arsenic in chloride slag is separated, obtains alkaline leaching slag, acid then is carried out to alkaline leaching slag again
Property leaching process, to separate copper therein, so as to obtain the acidic leaching residue of enriching noble metals.Copper anode mud provided by the invention
Preprocess method, it carries out pyrogenic process chlorination by using rotary kiln or fluidized roaster to copper anode mud so that after chlorination
Selenium, tellurium chloride-sublimation and enter flue gas, separated with chloride slag, the removing of selenium and tellurium is complete, solves selenium and tellurium whole
Scattering problem in copper anode slime treatment process, reduce and even avoid the influence of selenium, tellurium metal to gold and silver product quality, and
Such a mode of operation also allows for the centralized recovery of selenium and tellurium.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the process flow diagram of the preprocess method of copper anode mud provided in an embodiment of the present invention.
Embodiment
The invention provides a kind of preprocess method of copper anode mud, it can be by selenium, tellurium fully and the separation concentrated, drop
It is low or even avoid the influence of selenium, tellurium metal to gold and silver product quality.
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not made
Embodiment, belong to the scope of protection of the invention.
As shown in figure 1, the preprocess method of copper anode mud provided by the invention, using the joint metallurgy side of pyrogenic process-wet method
Method pre-processes to copper anode mud, and it comprises the following steps：
S101, copper anode mud is filtered successively, dry and ball-milling treatment：
Copper anode mud is put into the baking groove of baking oven and dried, 100 DEG C~105 DEG C of drying temperature, be incubated 2 hours~3 hours；
Ball milling, ball milling 1 hour~3 hours will be carried out through dry copper anode mud, until the earth of positive pole disperses soilless sticking.
S102 and then copper anode mud is added in rotary kiln or fluidized roaster progress pyrogenic process chlorination, will reaction
Obtained selenium and the chloride of tellurium is separated in the form of flue dust with copper anode mud：
Copper anode mud, which adds, carries out pyrogenic process chlorination in rotary kiln or fluidized roaster, at a temperature of 300 DEG C~500 DEG C,
When being passed through chlorine or adding chloride, larger chlorination occurs for selenium (tellurium) compound such as MeSe (Te), Me2Se (Te) anti-in the earth of positive pole
Should, generate corresponding chloride SeCl2, CuCl2, AgCl；The chloride of selenium and tellurium enters flue gas due to volatile, from flue gas
In can receive to obtain selenium-rich, the flue dust of tellurium chloride, slag enters alkaline leaching after chlorination.The main chemical reactions of generation are as follows：
ΜeSe(Τe)+2Cl2==ΜeCl2+Se(Τe)Cl2↑
Μe2Se(Τe)+3Cl2==2ΜeCl2+Se(Τe)Cl2↑。
S103, alkaline leaching processing is carried out to copper anode mud again, obtain alkaline leaching liquid and alkaline leaching slag：
Copper anode mud after chlorination is 1molL with concentration in retort-1~3molL-1Sodium hydroxide solution slurry
Change, liquid-solid ratio（L/kg）For 4:1~8:1, in temperature 70 C~90 DEG C, mixing speed 300rmin-1~500rmin-1's
Under the conditions of leach 2 hours~5 hours；Start to cool after reaching the reaction time, when temperature is reduced to less than 65 DEG C, releasing slurry is simultaneously
Separation of solid and liquid, obtains alkaline leaching liquid and alkaline leaching slag, alkaline leaching liquid recovery arsenic, and alkaline leaching slag enters acidic leaching.
The main chemical reactions of generation are as follows：
Αs2Ο3+2ΝaΟΗ+Ο2↑==2ΝaΑsΟ3+Η2Ο。
S104, acidic leaching processing finally is carried out to alkaline leaching slag, obtain the acid of acid leaching solution and enriching noble metals
Property leached mud, pretreatment operation complete：
In retort it is 1.5molL with concentration by alkaline leaching slag obtained in the previous step-1~4molL-1Sulfuric acid
Solution pulp, liquid-solid ratio（L/kg）For 4:1~8:1, in temperature 70 C~90 DEG C, mixing speed 250rmin-1~550r
min-1Under conditions of leach 2 hours~5 hours；Slurry and separation of solid and liquid are released after reaching the reaction time, obtains acid leaching solution
And acidic leaching residue, acid leaching solution recovery copper, acidic leaching residue recovery noble metal.The chemical reaction mainly occurred is as follows：
CuΟ+Η2SΟ4==CuSΟ4+Η2Ο
CuCl2+Η2SΟ4==CuSΟ4+Η2Ο
Cu(ΟΗ)2+Η2SΟ4==CuSΟ4+2Η2Ο。
In the preprocess method of copper anode mud provided by the invention, segment processing is carried out to copper anode mud, first to copper anode
Mud is filtered, dry and ball milling, then carries out pyrogenic process chlorination, chlorination to copper anode mud using rotary kiln or fluidized roaster
Selenium, the tellurium chloride obtained afterwards evaporates into flue dust state in rotary kiln or fluidized roaster and entered in flue gas, so as to
Realize the copper anode mud with solid-state（Copper anode mud now is referred to as chloride slag）It is abundant, concentrate separation, chloride slag is again
Handled by alkaline leaching, the arsenic in chloride slag is separated, obtains alkaline leaching slag, acid then is carried out to alkaline leaching slag again
Property leaching process, to separate copper therein, so as to obtain the acidic leaching residue of enriching noble metals.
The preprocess method of copper anode mud provided by the invention, it is by using rotary kiln or fluidized roaster to copper sun
Pole mud carries out pyrogenic process chlorination so that selenium, tellurium chloride-sublimation after chlorination and enter flue gas, separated with chloride slag, selenium and tellurium
Removing is complete, solves the scattering problem of selenium and tellurium in whole copper anode slime treatment process, reduces and even avoids selenium, tellurium gold
Belong to the influence to gold and silver product quality, and such a mode of operation also allows for the centralized recovery of selenium and tellurium.
In addition, chloride slag carries out alkaline leaching by sodium hydroxide, under suitable reaction condition, arsenic is with arsenic acid in chloride slag
The form of salt enters alkaline leaching liquid, and the leaching rate of arsenic reaches more than 98%, and arsenic removal effect is good；Alkaline leaching slag passes through sulfuric acid
When carrying out acidic leaching, the leaching rate of copper reaches more than 97%, and acid leaching solution is impure few, beneficial to subsequent handling processing；Using
Pyrogenic process-wet method combined metallurgical method, Purity of Noble Metals height, synthetical recovery high efficiency, good operational environment.
Embodiment 1
Copper anode mud is put into the baking groove of baking oven and dried, ball milling will be carried out through drying anode mud, until copper anode mud point
Soilless sticking is dissipated, is then stored standby.Dry copper anode mud main component is (%) by percentage to the quality:Au0.51、
Ag4.24, Cu10.52, Pb28.33, As4.17, Sb1.07, Se2.89 and Te0.36.
The above-mentioned copper anode muds of 200g are added to progress pyrogenic process chlorination in fluidized roaster, 350 DEG C is to slowly warm up to, leads to
Enter excessive chlorine, keep reacting 2h under pressure 0.6MPa, after reaching the reaction time, collection flue dust to be cooled, take out chloride slag, chlorine
Slugging is weighed as 139.6g, and its main component is (%) by percentage to the quality:Au0.73、Ag6.03、Cu15.02、Pb40.49、
As5.89, Sb1.48, Se0.034 and Te0.0038.
1.5mol/L sodium hydroxide solution 500ml are prepared, are added in the reactor for filling the above-mentioned chloride slags of 120g, in temperature
75 DEG C, mixing speed 350rmin-1Under conditions of leach 2h；Start to cool after reaching the reaction time, when temperature is reduced to 65 DEG C
Slurry and separation of solid and liquid are released below, obtain alkaline leaching liquid and alkaline leaching slag, alkaline leaching pulp water is dried after washing weighs, alkali
Property leached mud weight 87.25g, its main component is (%) by percentage to the quality:Au0.97、Ag8.23、Cu20.51、Pb55.24、
As0.049, Sb1.97, Se0.046 and Te0.0051, the leaching rate of arsenic is 99.39%.
The sulfuric acid solution pulp for being 2mol/L with concentration in reactor by 80g alkaline leaching slags obtained in the previous step,
80 DEG C of temperature, mixing speed 300rmin-1Under conditions of leach 2.5h；Slurry and separation of solid and liquid are released after reaching the reaction time,
Acid leaching solution and acidic leaching residue are obtained, dries and weighs after acidic leaching residue washing, acidic leaching residue weight 55.24g, its is main
Composition is (%) by percentage to the quality:Au1.38, Ag11.69, Cu0.22, Pb78.23, As0.07, Sb2.76, Se0.063 and
Te0.0071, the leaching rate of copper is 99.26%.
Embodiment 2
Copper anode mud is filtered by filter press, copper anode mud is put into the baking groove of baking oven after filtering and dried, will be through dry
Dry copper anode mud carries out ball milling, until copper anode mud disperses soilless sticking, then stores standby.Copper anode mud main component is with matter
It is (%) to measure percentages:Au0.23, Ag2.83, Cu7.18, Pb23.45, As3.15, Sb0.76, Se3.54 and Te0.61.
The above-mentioned copper anode muds of 200g are added to progress pyrogenic process chlorination in rotary kiln or fluidized roaster, are to slowly warm up to
450 DEG C, excessive chlorine is passed through, keeps reacting 2h under pressure 0.7MPa, after reaching the reaction time, collection flue dust to be cooled, takes out
Chloride slag, chloride slag are weighed as 132.7g, and its main component is (%) by percentage to the quality:Au0.34、Ag4.19、
Cu10.55, Pb35.14, As4.63, Sb1.08, Se0.028 and Te0.0044.
2.5mol/L sodium hydroxide solution 500ml are prepared, are added in the reactor for filling the above-mentioned chloride slags of 120g, in temperature
85 DEG C, mixing speed 450rmin-1Under conditions of leach 2h；Start to cool after reaching the reaction time, when temperature is reduced to 65 DEG C
Slurry and separation of solid and liquid are released below, obtain alkaline leaching liquid and alkaline leaching slag, alkaline leaching pulp water is dried after washing weighs, alkali
Property leached mud weight 82.16g, its main component is (%) by percentage to the quality:Au0.49、Ag5.96、Cu15.23、Pb50.32、
As0.04, Sb1.52, Se0.038 and Te0.0062, the leaching rate of arsenic is 99.41%.
The sulfuric acid solution pulp for being 3mol/L with concentration in reactor by 80g alkaline leaching slags obtained in the previous step,
Temperature 70 C, mixing speed 400rmin-1Under conditions of leach 3.5h；Slurry and separation of solid and liquid are released after reaching the reaction time,
Acid leaching solution and acidic leaching residue are obtained, dries and weighs after acidic leaching residue washing, acidic leaching residue weight 52.61g, its is main
Composition is (%) by percentage to the quality:Au0.73, Ag8.92, Cu0.16, Pb75.52, As0.059, Sb2.21, Se0.056 and
Te0.0091, the leaching rate of copper is 99.32%.
Each embodiment is described by the way of progressive in this specification, what each embodiment stressed be and other
The difference of embodiment, between each embodiment identical similar portion mutually referring to.
The foregoing description of the disclosed embodiments, professional and technical personnel in the field are enable to realize or using the present invention.
A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope caused.
Claims (5)
1. a kind of preprocess method of copper anode mud, it is characterised in that comprise the following steps：
1) copper anode mud is filtered successively, dry and ball-milling treatment；
2) progress pyrogenic process chlorination in rotary kiln or fluidized roaster and then by the copper anode mud is added to, reaction is obtained
Selenium and the chloride of tellurium separated in the form of flue dust with the copper anode mud containing noble metal, when carrying out pyrogenic process chlorination,
Temperature in the rotary kiln or fluidized roaster is 300 DEG C~500 DEG C；
3) alkaline leaching processing is carried out to the copper anode mud again, obtains alkaline leaching liquid and alkaline leaching slag；
4) acidic leaching processing finally is carried out to the alkaline leaching slag, obtains the acid leaching of acid leaching solution and enriching noble metals
Slag tap.
2. the preprocess method of copper anode mud according to claim 1, it is characterised in that done to the copper anode mud
During dry processing, drying temperature is 100 DEG C~105 DEG C, and is incubated 2~3 hours to the copper anode mud.
3. the preprocess method of copper anode mud according to claim 1, it is characterised in that ball is carried out to the copper anode mud
During mill processing, Ball-milling Time is 1 hour~3 hours.
4. the preprocess method of copper anode mud according to claim 1, it is characterised in that carrying out alkaline leaching processing
When, the copper anode mud after chlorination is 1molL with concentration in retort-1~3molL-1Sodium hydroxide solution slurry
Change, liquid-solid ratio 4:1~8:1, in temperature 70 C~90 DEG C, leach 2 hours~5 hours；Cooled after reaching the reaction time,
When temperature is reduced to less than 65 DEG C, slurry and separation of solid and liquid are released, obtains alkaline leaching liquid and alkaline leaching slag.
5. the preprocess method of the copper anode mud according to any one in claim 1-4, it is characterised in that carrying out acid
During property leaching process, the alkaline leaching slag is 1.5molL with concentration in retort-1~4molL-1Sulfuric acid solution
Pulp, liquid-solid ratio 4:1~8:1, in temperature 70 C~90 DEG C, leach 2 hours~5 hours；Slurry is released after reaching the reaction time
Expect simultaneously separation of solid and liquid, obtain the acidic leaching residue of acid leaching solution and enriching noble metals.
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