CN204570063U - Hydrometallurgy galvanic deposit operation porous aluminum based composite anode - Google Patents
Hydrometallurgy galvanic deposit operation porous aluminum based composite anode Download PDFInfo
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- CN204570063U CN204570063U CN201520133758.2U CN201520133758U CN204570063U CN 204570063 U CN204570063 U CN 204570063U CN 201520133758 U CN201520133758 U CN 201520133758U CN 204570063 U CN204570063 U CN 204570063U
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Abstract
The utility model discloses a kind of hydrometallurgy galvanic deposit operation porous aluminum based composite anode.Described anode substrate is for having the aluminium alloy of " three-dimensional through hole structure ", on the hole wall of " the three-dimensional through hole structure " of alloy matrix aluminum and aluminium alloy matrix surface be provided with coating layer, described coating layer is made up of pb-ag alloy internal layer and the hydrometallurgy electrodeposition operation lead alloy skin of ripe lead anode; Its preparation method comprises: the pre-treatment of porous aluminum matrix, pb-ag alloy bottom on porous aluminum matrix be accompanied by and the large step of aftertreatment three.The utility model porous aluminum based composite anode is lightweight, has low overpotential for oxygen evolution, good electroconductibility and creep resistance, aluminium/plumbous interface cohesion are tight, adopts this anode to produce cathode product quality high, anode manufacture adopt the cost of raw material low; Be suitable for large-scale industrial to produce.
Description
Technical field
The utility model relates to a kind of hydrometallurgy galvanic deposit operation porous aluminum based composite anode, belongs to technical field of wet metallurgy.
Background technology
Due to hydrometallurgy have that comprehensive resource utilization rate is high, process environmental protection and to advantages such as low grade ore strong adaptabilities, the non-ferrous metals such as Cu, Zn, Ni, Co, Cd, Mn are undertaken extracting the share accounted for by wet method and increase gradually.Galvanic deposit is the important procedure that hydrometallurgy extracts in non-ferrous metal technological process, the insoluble Pb alloy of current industrial most employing is as anode, but because lead density is large, specific conductivity is not high and tensile strength is little, thus cause anode in use easily to occur the appearance of the defects such as the large and current efficiency of creep, anode drop is low; In addition, the silver also containing many content in some anode, result also in anode material cost high.Therefore alleviate anode weight, improve anode conductivity and tensile strength, to reduce the lifting of bullion content to existing hydrometallurgical technology in anode significant.
To be combined with each other that to prepare aluminium base plumbous composite anode be the effective means improving anode performance with aluminium by plumbous, forefathers also do a lot in this respect.Patent 200710065927.3 and patent 01135605.7 have employed similar method, namely the mode of dipping or electroless plating of first passing through is at aluminum surface layer preplating one deck transition metal layer, and then casting lead alloy is carried out on pre-plating layer, zone of oxidation due to aluminium surface is easy to be formed, and these class methods certainly will be difficult to ensure the long-acting combination of card pre-plating layer and aluminum substrate.Patent 200910094290.X discloses a class directly method of lead plating alloy layer on aluminum substrate, and the method is except complex process, and the control of thickness of coating and the combination between coating and aluminum substrate are still its subject matter.
Develop aluminium base plumbous composite anode for prior art and there is aluminum substrate and lead alloy top layer is difficult to the aspect problems such as long-acting combination and complex process, the present inventor, through repeatedly studying, has invented a kind of hydrometallurgy galvanic deposit operation porous aluminum-base composite lead anode.
Utility model content
The purpose of this utility model is the deficiency overcoming prior art, provides a kind of rational in infrastructure, electroconductibility and creep-resistant property is good, long service life, aluminium/plumbous interface cohesion hydrometallurgy galvanic deposit closely operation porous aluminum based composite anode.
A kind of hydrometallurgy galvanic deposit operation of the utility model porous aluminum based composite anode, described composite anode matrix is for having the aluminium alloy of " three-dimensional through hole structure ", on the hole wall of " the three-dimensional through hole structure " of alloy matrix aluminum and aluminium alloy matrix surface be provided with coating layer, described coating layer is made up of pb-ag alloy internal layer and the hydrometallurgy electrodeposition operation lead alloy skin of ripe lead anode;
A kind of hydrometallurgy galvanic deposit operation of the utility model porous aluminum based composite anode, in alloy matrix aluminum, the clear size of opening of " three-dimensional through hole structure " is 4-8mm, and the porosity of alloy matrix aluminum is 60-80%;
A kind of hydrometallurgy galvanic deposit operation of the utility model porous aluminum based composite anode, in coating layer, the thickness of internal layer pb-ag alloy is 0.2-0.5mm, and the thickness of outer lead alloy is 0.8-2.5mm; In pb-ag alloy, the mass percentage of silver is 0.2-0.6wt%.
A kind of hydrometallurgy galvanic deposit operation of the utility model porous aluminum based composite anode, in alloy matrix aluminum, the mass percentage of each element is:
0.5-1.5wt%Mg, 3-5wt%Si, 0.5-1.5wt%Cu, aluminium surplus.
A kind of hydrometallurgy galvanic deposit operation of the utility model porous aluminum based composite anode, anode hole is of a size of 1-2mm, and the porosity of anode is 55-65%.
The preparation method of a kind of hydrometallurgy galvanic deposit of the utility model operation porous aluminum based composite anode, comprises the steps:
The first step: alloy matrix aluminum pre-treatment
Select hole to be interconnected, bore hole size be 4-8mm, porosity is the alloy matrix aluminum of 60-80%,
By alloy matrix aluminum, being placed in temperature is that the nitric acid vapor of 60-100 DEG C is oxidized, after surface produces micropore, and washing; Then, the alloy matrix aluminum after oxidation is placed in sodium hydroxide lye and soaks, the micropore that nitric acid oxidation is formed expands, finally, with deionized water rinsed clean, oven dry;
Second step: the coated pb-ag alloy of aluminium alloy matrix surface
By the first step gained alloy matrix aluminum and pb-ag alloy ingot one packaged enter encloses container, encloses container is evacuated down to 0.01-10Pa, then, maintain vacuum tightness, after encloses container being warmed up to 350-520 DEG C of insulation 10-30min, in encloses container, pass into rare gas element, make the pressure of encloses container reach 15-120Mpa, after pressurize 30-60mi; Cool to 320-330 DEG C with stove, release, at this temperature, alloy matrix aluminum is taken out in plumbous melt, air-cooled, obtain the porous anode crude green body that surface bonding has pb-ag alloy layer;
3rd step: aftertreatment is carried out to the first base of second step gained porous anode
After second step gained anode crude green body surface chemistry terne coating, be in the lead alloy melt of the ripe lead anode of hydrometallurgy electrodeposition operation of 350-450 DEG C, carry out at least 3 recycle metal baths in temperature, obtain hydrometallurgy galvanic deposit operation porous aluminum based composite anode.
In the preparation method of a kind of hydrometallurgy galvanic deposit of the utility model operation porous aluminum based composite anode, alloy matrix aluminum is oxidized in nitric acid vapor, be by unsettled for the alloy matrix aluminum salpeter solution liquid level in closed reactor, heating salpeter solution is oxidized alloy matrix aluminum; The mass percentage concentration of described salpeter solution is 65-68%, and its volume accounts for the 5-30% of closed reactor volume, oxidization time 5-30min;
In sodium hydroxide lye, sodium hydrate content is 40-60g/l, and the temperature of sodium hydroxide lye is 40-55 DEG C, soak time 5-10min.
In the preparation method of a kind of hydrometallurgy galvanic deposit of the utility model operation porous aluminum based composite anode, when lowering the temperature with stove, in maintenance encloses container, pressure is at 15-120Mpa, and rate of temperature fall is 1-5 DEG C/min.
In the preparation method of a kind of hydrometallurgy galvanic deposit of the utility model operation porous aluminum based composite anode, surface chemistry terne coating, that first for porous anode base is placed in chemical plating fluid, at 75-100 DEG C of (preferably 90 DEG C) temperature, react 20-60min (preferred 30min), in chemical plating fluid, the content of each component is:
Methylsulphonic acid 150-350ml/l (preferred 200ml/l),
Tin methane sulfonate 200-400ml/l (preferred 320ml/l),
The plumbous 100-300ml/l (preferred 160ml/l) of methylsulphonic acid,
Thiocarbamide 50-100g/l (preferred 80g/l),
Sodium hypophosphite 5-15g/l (preferred 10g/l),
EDTA1-3g/l (preferred 2g/l),
Xitix 1-3g/l (preferred 2g/l).
Adopt the preparation method of composite anode described in the utility model, " long-acting seamless " that can realize between aluminum substrate and lead alloy combines, reason is as follows: when 1. carrying out pre-treatment to porous aluminum matrix, acid gas atmosphere and dilute alkaline soln dual corrosion, this not only can remove the oxide skin on porous aluminum surface, particularly by nitric acid vapor to core surfaces corrosion treatment, can corrosion hole be produced, during follow-up alkaline purification, due to Al
2o
3can react with alkali with Al, expand aluminium surface micropore size further, be conducive to pb-ag alloy melt and immerse in the micropore of aluminium alloy matrix surface, subsequently, adopt the infiltration applying certain pressure in encloses container, utilize impressed pressure, overcome aluminium, plumbous interface wettability is poor, the obstacle that plumbous melt is not easily combined with aluminum alloy surface, pb-ag alloy melt can be immersed in the micropore of aluminium alloy matrix surface, then, near lead alloy melting temperature, alloy matrix aluminum takes out by (320-330 DEG C) from pb-ag alloy melt, air-cooled, make the pb-ag alloy quick solidification sticking to aluminium alloy matrix surface, immerse the pb-ag alloy in aluminum alloy surface micropore and form mechanical snap between micropore, realize the physical bond of pb-ag alloy and alloy matrix aluminum, 2. in the aluminium alloy that the utility model alloy matrix aluminum is selected, master alloying element is Mg, at about 350-520 DEG C, when pressurization, insulation, the lead of molten state and magnesium form Mg-Pb or Al-Mg-Pb alloy, realize " metallurgical binding " at aluminium alloy core matrix/plumbous interface.The utility model has the alloy matrix aluminum of three-dimensional through hole by arranging, master alloying element is selected to be the aluminium alloy of magnesium, the combination of rapid air-cooled technique after employing pressure infiltration, make between composite anode top layer lead alloy and core aluminium alloy, to form " physical bond " and " metallurgical binding ", guarantee that " long-acting seamless " between aluminum substrate and lead alloy combines.There is the defect that aluminum substrate and lead alloy top layer are difficult to long-acting combination and complex process in the aluminium base plumbous composite anode overcome prepared by prior art.
Subsequently, learn terne coating and recycle metal bath on pb-ag alloy surface, the ripe lead anode lead alloy being applicable to hydrometallurgy electrodeposition operation at pb-ag alloy surface parcel is outer, prepares porous porous aluminum-base composite anode.
The electroconductibility of the utility model composite anode and physical strength are all good, mainly because the constituent class of adopted foamed aluminium radical system aluminium alloy for subsequent use is similar to ZL101A, there are some researches show (see " Special Processes of Metal Castings and non-ferrous alloy; 2010; 30 [12]: 1162-1165 "), the specific conductivity of such alloy 20 DEG C time is 23.20-23.78MSm
-1, the tensile strength after T6 process can reach 285MPa, namely aluminium alloy specific conductivity close to plumbous 5 times, tensile strength is close to 15 times of high-strength lead alloy; In addition, anode adopts vesicular structure, by controlling its porosity, under the prerequisite ensureing anode strength property, anode weight is greatly alleviated, and the anode of preparation has outstanding creep-resistant property and lightweight.
The utility model develop the positively effect that anode has low overpotential for oxygen evolution, long life and high-quality cathode product, this is because: 1. " the three-dimensional through hole structure " of anode makes the conductive surface area comparatively classic flat-plate anode increase a lot of times of its reality, thus the actual current density of anode is greatly reduced, according to Tafel equation η=a+blogi, reduce the reduction that current density can realize oxygen overpotential on anode; 2. under low current density, electrodeposition process Anodic surface institute formed oxide film densification, effectively can improve the acid corrosion-resistant performance of anode, this not only reduces anode lead and to be corroded the speed entering electrolytic solution, the lead content reduced in cathode product, but also effectively extend anode life.
The material cost (particularly bullion content) of the utility model composite anode more industrial anode used significantly reduces, and this is mainly caused by unique vesicular structure of anode and high porosity.
Therefore, the utility model composite anode, compared with anode that known technology is announced, has following major advantage and positively effect:
(1) prepared by the utility model technology, anode has good electroconductibility and creep resistance, and this will be conducive to the reduction of bath voltage and reduce anode in short circuit number of times, thus can realize the saving of electrodeposition process energy consumption;
(2) vesicular structure of anode, makes the actual current density flowing through anode greatly reduce, this be anodic overpotential significantly reduction, save galvanic deposit power consumption and lay a good foundation further; Low current density can make the passive film of anode surface finer and close, and this is very beneficial for extending anode life and improving cathode product quality;
(3) vesicular structure of anode not only makes that quality of anode significantly alleviates, the lead alloy raw material of anode manufacture significantly reduces, and labour intensity when effectively alleviating workman's change poles plate.
In addition, the porous aluminum pre-treatment adopting the utility model to limit also in conjunction with vacuum pressure infiltration, can realize aluminium/plumbous interface " long-acting seamless " and combine, and avoids the appearance that the methods such as traditional plating may cause existing defect such as plating dead angle, trachoma etc.
Accompanying drawing explanation
Accompanying drawing 1 is the structural representation of the utility model porous al base sacrificial anode;
Accompanying drawing 2 is I enlarged view in accompanying drawing 1;
In figure: 000---hole, 001---alloy matrix aluminum, 002---pb-ag alloy internal layer, 003---lead alloy is outer, 001---hole wall.
Embodiment
Below in conjunction with accompanying drawing, the utility model is described in further detail, but the utility model is not limited thereto.
See accompanying drawing 1,2.
The preparation of porous al base sacrificial anode of embodiment 1 Zinc electrolysis
A kind of hydrometallurgy galvanic deposit operation porous aluminum based composite anode, described composite anode matrix is for having the aluminium alloy of " three-dimensional through hole structure ", at the hole wall (001) of " the three-dimensional through hole structure " of alloy matrix aluminum (001), upper and aluminium alloy matrix surface is provided with coating layer, and described coating layer is made up of pb-ag alloy internal layer (002) and the hydrometallurgy electrodeposition operation lead alloy skin (003) of ripe lead anode; In alloy matrix aluminum, the through hole (000) of " three-dimensional through hole structure " is of a size of 4-6mm, and the porosity of alloy matrix aluminum is 60%; In coating layer, the thickness of internal layer pb-ag alloy is 0.3mm, and the thickness of outer lead alloy is 1mm; Mass percentage silver-colored in pb-ag alloy is the mass percentage of each element in 0.2-0.6wt% alloy matrix aluminum:
0.5wt%Mg, 3wt%Si and 0.5wt%Cu, aluminium surplus.
Anode hole is of a size of 1-2mm, and the porosity of anode is 55-65%.
Its preparation method, comprises the steps:
The first step: alloy matrix aluminum pre-treatment
Select hole to be interconnected, bore hole size be 4-8mm, porosity is the alloy matrix aluminum of 60-80%,
By alloy matrix aluminum, on unsettled salpeter solution liquid level in closed reactor, heating salpeter solution to 100 DEG C, produces nitric acid vapor and is oxidized alloy matrix aluminum, oxidization time 5min, after surface produces micropore (102), and washing; Then, the alloy matrix aluminum after oxidation being placed in sodium hydrate content is that the sodium hydroxide lye of 60g/l soaks 5min, and the temperature of sodium hydroxide lye is 55 DEG C, and the micropore expansion that nitric acid oxidation is formed, finally, with deionized water rinsed clean, oven dry;
The mass percentage concentration of described salpeter solution is 66%, and its volume accounts for 5% of closed reactor volume;
Second step: the coated pb-ag alloy of aluminium alloy matrix surface
By packaged for the pb-ag alloy ingot one of the first step gained alloy matrix aluminum and silver content 0.2wt% enter encloses container, encloses container is evacuated down to 0.01Pa, then, maintain vacuum tightness, after encloses container being warmed up to 520 DEG C of insulation 40min, in encloses container, pass into rare gas element, make the pressure of encloses container reach 60Mpa, after pressurize 60mi; Keep pressure in encloses container constant, rate of temperature fall is 2 DEG C/min, cools to 320 DEG C with stove, release, at this temperature, slowly takes out alloy matrix aluminum in plumbous melt, air-cooled, obtain the porous anode crude green body (200) that surface bonding has pb-ag alloy layer;
3rd step: aftertreatment is carried out to the first base of second step gained porous anode
Chemical plating fluid is placed in second step gained anode crude green body, react 25min at 80 DEG C of temperature after, be in the lead alloy melt of the ripe lead anode of hydrometallurgy electrodeposition operation of 350 DEG C, carry out 3 minor metal bath circulations in temperature, obtain hydrometallurgy galvanic deposit operation porous aluminum based composite anode (300);
In chemical plating fluid, the content of each component is:
Methylsulphonic acid 200ml/l,
Tin methane sulfonate 320ml/l,
The plumbous 150ml/l of methylsulphonic acid,
Thiocarbamide 80g/l,
Sodium hypophosphite 10g/l,
EDTA 2g/l，
Xitix 2g/l.
Quantitative measurement result shows: in anode prepared by the present embodiment, silver content is 0.13%, only has industrial 16% of current zinc hydrometallurgy Pb-Ag (0.8wt%) anode; Specific conductivity 5.85MSm
-1, exceed dull and stereotyped Pb-Ag (0.8wt%) anode 20%; Tensile strength 42.5MPa, is equivalent to 2 times of dull and stereotyped alloy lead anode.Found by porous base anode described in contrast the present embodiment and the electrodeposition behavior of dull and stereotyped Pb-Ag (0.8wt%) anode under the industrial electrolysis condition of Zinc electrolysis: the more dull and more stereotyped Pb-Ag of overpotential for oxygen evolution (0.8wt%) anode of porous al base sacrificial anode reduces 148mV; Corrosion rate in electrolyte system is only 20% of dull and stereotyped anode; Lead content in cathode product zinc is 0.00079%, is only dull and stereotyped anode gained cathode product 51%.These test results show, the over-all properties of the utility model anode is far superior to traditional dull and stereotyped lead anode.
The preparation of porous al base sacrificial anode of embodiment 2 bronze medal electrodeposition
A kind of hydrometallurgy galvanic deposit operation porous aluminum based composite anode, described composite anode matrix is for having the aluminium alloy of " three-dimensional through hole structure ", at the hole wall (011) of " the three-dimensional through hole structure " of alloy matrix aluminum (001), upper and aluminium alloy matrix surface is provided with coating layer, and described coating layer is made up of pb-ag alloy internal layer (002) and the hydrometallurgy electrodeposition operation lead alloy skin (003) of ripe lead anode; In alloy matrix aluminum, the through hole (000) of " three-dimensional through hole structure " is of a size of 5-8mm, and the porosity of alloy matrix aluminum is 70%; In coating layer, the thickness of internal layer pb-ag alloy is 0.3mm, and the thickness of outer lead alloy is 1.2mm; Mass percentage silver-colored in pb-ag alloy is the mass percentage of each element in 0.2-0.6wt% alloy matrix aluminum:
0.9wt%Mg, 4wt%Si and 1wt%Cu, aluminium surplus.
Anode hole is of a size of 1-2mm, and the porosity of anode is 55-65%.
Its preparation method, comprises the steps:
The first step: alloy matrix aluminum pre-treatment
Select hole to be interconnected, bore hole size be 4-8mm, porosity is the alloy matrix aluminum of 60-80%,
By alloy matrix aluminum, on unsettled salpeter solution liquid level in closed reactor, heating salpeter solution to 60 DEG C, produces nitric acid vapor and is oxidized alloy matrix aluminum, oxidization time 8min, after surface produces micropore (102), and washing; Then, the alloy matrix aluminum after oxidation being placed in sodium hydrate content is that the sodium hydroxide lye of 40g/l soaks 10min, and the temperature of sodium hydroxide lye is 45 DEG C, and the micropore expansion that nitric acid oxidation is formed, finally, with deionized water rinsed clean, oven dry;
The mass percentage concentration of described salpeter solution is 66%, and its volume accounts for 30% of closed reactor volume;
Second step: the coated pb-ag alloy of aluminium alloy matrix surface
By packaged for the pb-ag alloy ingot one of the first step gained alloy matrix aluminum and silver content 0.6wt% enter encloses container, encloses container is evacuated down to 1Pa, then, maintain vacuum tightness, after encloses container being warmed up to 520 DEG C of insulation 30min, in encloses container, pass into rare gas element, make the pressure of encloses container reach 90Mpa, after pressurize 45mi; Keep pressure in encloses container constant, rate of temperature fall is 5 DEG C/min, cools to 330 DEG C with stove, release, at this temperature, slowly takes out alloy matrix aluminum in plumbous melt, air-cooled, obtain the porous anode crude green body (200) that surface bonding has pb-ag alloy layer;
3rd step: aftertreatment is carried out to the first base of second step gained porous anode
Chemical plating fluid is placed in second step gained anode crude green body, react 30min at 90 DEG C of temperature after, be in the lead alloy melt of the ripe lead anode of hydrometallurgy electrodeposition operation of 350 DEG C, carry out 6 minor metal bath circulations in temperature, obtain hydrometallurgy galvanic deposit operation porous aluminum based composite anode (300);
In chemical plating fluid, the content of each component is:
Methylsulphonic acid 200ml/l,
Tin methane sulfonate 320ml/l,
The plumbous 150ml/l of methylsulphonic acid,
Thiocarbamide 80g/l,
Sodium hypophosphite 10g/l,
EDTA 2g/l，
Xitix 2g/l.
Quantitative measurement result shows: in anode prepared by the present embodiment, silver content is 0.04%, specific conductivity 5.46MSm
-1, exceed dull and stereotyped Pb-Ag (0.8wt%) anode 12%; Tensile strength 34.5MPa, is equivalent to 1.5 times of dull and stereotyped alloy lead anode.By porous base anode described in comparative analysis the present embodiment and classic flat-plate Pb-Ca-Sn anode, behavior in copper electrodeposition finds, the more dull and more stereotyped anode of overpotential for oxygen evolution of porous al base sacrificial anode reduces 128mV; Corrosion rate in electrolyte system is only 25% of dull and stereotyped anode; Lead content in cathode product copper is only dull and stereotyped anode gained cathode product 51%.These test results show, the over-all properties of the utility model anode is far superior to traditional dull and stereotyped lead anode.
Claims (5)
1. hydrometallurgy galvanic deposit operation porous aluminum based composite anode, it is characterized in that: described composite anode matrix is for having the aluminium alloy of " three-dimensional through hole structure ", on the hole wall of " the three-dimensional through hole structure " of alloy matrix aluminum and aluminium alloy matrix surface be provided with coating layer, described coating layer is made up of pb-ag alloy internal layer and the hydrometallurgy electrodeposition operation lead alloy skin of ripe lead anode.
2. composite anode according to claim 1, is characterized in that: in alloy matrix aluminum, the clear size of opening of " three-dimensional through hole structure " is 4-8mm, and the porosity of alloy matrix aluminum is 60-80%.
3. composite anode according to claim 1, it is characterized in that: in coating layer, the thickness of internal layer pb-ag alloy is 0.2-0.5mm, the thickness of outer lead alloy is 0.8-2.5mm.
4. composite anode according to claim 3, is characterized in that: in pb-ag alloy, the mass percentage of silver is 0.2-0.6wt%.
5. composite anode according to claim 1-4 any one, is characterized in that: anode hole is of a size of 1-2mm, and the porosity of anode is 55-65%.
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| CN104762639A (en) * | 2015-03-09 | 2015-07-08 | 中南大学 | A porous aluminum-based composite anode used for a hydrometallurgy electrodeposition process and a preparing method |
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| CN104762639A (en) * | 2015-03-09 | 2015-07-08 | 中南大学 | A porous aluminum-based composite anode used for a hydrometallurgy electrodeposition process and a preparing method |
| CN104762639B (en) * | 2015-03-09 | 2017-03-15 | 中南大学 | Hydrometallurgy electro-deposition operation porous aluminum based composite anode and preparation method |
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Effective date of registration: 20210302 Address after: No. 1299, Changyuan North Road, high tech Zone, Kunming, Yunnan 650000 Patentee after: KUNMING HENDERA SCIENCE AND TECHNOLOGY Co.,Ltd. Address before: 410083 Hunan province Changsha Lushan Road No. 1 Patentee before: CENTRAL SOUTH University |
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