CN103526234B - Fused salt electrolysis process extracts the method for metal from flyash - Google Patents
Fused salt electrolysis process extracts the method for metal from flyash Download PDFInfo
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Abstract
Fused salt electrolysis process extracts the method for metal from flyash, belongs to metallurgical technology field, and method one is: (1) is by Na3AlF6And AlF3It is mixed and made into ice crystal ground mass fused salt；(2) it is placed in electrolysis bath and adds flyash；(3) heating is to 910 ~ 985 DEG C, is then electrified to carry out electrolysis, formation of deposits acieral on negative electrode。Method two is: (1) is by Na3AlF6And AlF3Mix homogeneously makes ice crystal ground mass fused salt；(2) it is placed in electrolysis bath and adds flyash and aluminium oxide；(3) heating to 930 ~ 985 DEG C, be then electrified to carry out electrolysis, electrolysis complete after on negative electrode formation of deposits acieral。The present invention passes through fused salt electrolysis process treated coal ash, and alloy is prepared in the direct electro-deposition of oxide such as aluminum, silicon, titanium and ferrum, it is achieved the green high-efficient comprehensive utilization of flyash, there is technique simple, can produce at existing industrial aluminum electrolysis bath, and flow process is short, the advantage that can be continuously produced。
Description
Technical field
The invention belongs to metallurgical technology field, particularly to the method that fused salt electrolysis process extracts metal from flyash。
Background technology
Flyash is commonly called as flying dust, refers to the dust and bottom slag collected from coal-fired (containing gangue, coal slime) boiler smoke and the desulphurization and denitration lime-ash produced in coal-burning power plant's production process。Flyash yield and discharge capacity are cumulative year after year trend, and accumulating over a long period of flyash substantially becomes public hazards。The main silica of chemical composition of flyash, aluminium sesquioxide, iron sesquioxide, calcium oxide, magnesium oxide, potassium oxide, sodium oxide, sulfur trioxide, loss on ignition etc.。
At present, the utilization of flyash is concentrated mainly on the aspect such as building materials and road construction work, and the extensive style substantially belonging to low value-added utilizes, and utilization ratio is not high。It addition, existing total utilization of PCA research work has focused largely in flyash in the recycling of bauxite resource。The method extracting aluminium oxide from flyash mainly has alkaline process, acidleach to follow the example of, using acid and alkali combination method and ammonium sulfate roasting method, but every kind of method all has respective deficiency。Wherein alkaline process mainly includes soda lime sintering process and limestone sintering process, and the alkali reaction agent of alkali process can not recycle, and energy consumption is high, and production cost is high, and the level of residue produced is big；Acid leaching process mainly adopts sulphuric acid or hydrochloric acid leaching flyash, also by Elements Leachings such as Fe, K, Mg, Ca, can increase the extraction difficulty of aluminium oxide, and equipment corrosion is serious during Acid leaching, and production cost is high；The alumina product quality that using acid and alkali combination method prepares is higher, but production process and equipment are many, and energy consumption is big, and production cost is high；Ammonium sulfate roasting method is by by baking mixed to flyash and ammonium sulfate, but still suffers from the problems such as energy consumption height, purification rate are low。Only embodying the recycling to bauxite resource in these research work, not yet real embodiment comprehensively utilizes the silicon oxide in flyash and aluminium oxide。
Summary of the invention
For the problems referred to above that existing recycling flyash exists technically, the present invention provides the method that fused salt electrolysis process extracts metal from flyash, using cryolite as flux, villiaumite is as additive, flyash is as raw material, by being dissolved in cryolite fused salt system, adopts carbon anode or inert anode as anode, at high temperature carry out the metal in electroextraction flyash, make acieral。
The fused salt electrolysis process of the present invention is extracted the method for metal from flyash and is divided into two kinds, and first method is to sequentially include the following steps:
1, by Na3AlF6And AlF3Mix homogeneously makes ice crystal ground mass fused salt, and mixed proportion presses NaF and the AlF in ice crystal ground mass fused salt3Mol ratio be 2 ~ 2.8；
2, being placed in electrolysis bath by ice crystal ground mass fused salt, be subsequently adding flyash, the addition of flyash is the 3 ~ 10% of ice crystal ground mass fused salt and flyash gross weight；
3, heating ice crystal ground mass fused salt and flyash to 910 ~ 985 DEG C, be then electrified to carry out electrolysis, the electric current density controlled between negative electrode and anode is 0.4 ~ 1.2A/cm2, electrolysis time is 3 ~ 8h, electrolysis complete after on negative electrode formation of deposits acieral。
In said method, the negative electrode adopted during electrolysis is aluminum liquid, and anode is carbon anode or inert anode, and described inert anode is metal base aluminium electrolytic inert anode。
In said method, when starting after electrolysis, per half an hour adds a flyash in electrolysis bath, when the fine coal ash quantity every time added is start electrolysis in electrolysis bath the 20 ~ 80% of flyash gross weight。
The composition of the acieral that said method deposits on negative electrode is by weight percentage containing Al67 ~ 76%, Si17 ~ 20%, Fe2.5 ~ 6.5%, Ti1 ~ 8.5%, and surplus is impurity。
The response rate of metal respectively Al50 ~ 80%, Si70 ~ 90%, Fe60 ~ 80%, Ti85 ~ 95% in flyash in said method。
Second method sequentially includes the following steps:
1, by Na3AlF6And AlF3Mix homogeneously makes ice crystal ground mass fused salt, and mixed proportion presses NaF and the AlF in ice crystal ground mass fused salt3Mol ratio be 2 ~ 2.8；
2, ice crystal ground mass fused salt is placed in electrolysis bath, it is subsequently adding the mixed material of flyash and aluminium oxide, in mixed material, flyash accounts for the 10 ~ 60% of mixed material gross weight, and all the other are aluminium oxide, and mixed material accounts for the 2 ~ 8% of ice crystal ground mass fused salt and mixed material gross weight；
3, heating ice crystal ground mass fused salt and mixed material to 930 ~ 985 DEG C, be then electrified to carry out electrolysis, the electric current density controlled between negative electrode and anode is 0.4 ~ 1.0A/cm2, electrolysis time is 3 ~ 8h, electrolysis complete after on negative electrode formation of deposits acieral。
In above-mentioned second method, the negative electrode adopted during electrolysis is aluminum liquid, and anode is carbon anode。
In above-mentioned second method, after starting electrolysis, per half an hour adds the mixed material of a flyash and aluminium oxide in electrolysis bath, and in mixed material, flyash accounts for the 10 ~ 60% of mixed material gross weight；The mixture doses every time added be start electrolysis time electrolysis bath in mixed material gross weight 20 ~ 80%。
The composition of the acieral that above-mentioned second method deposits on negative electrode is by weight percentage containing Al85 ~ 96%, Si2.5 ~ 12.5%, Fe0.8 ~ 1.6%, Ti0.3 ~ 2.5%, and surplus is impurity。
The response rate of metal respectively Al50 ~ 80%, Si70 ~ 90%, Fe60 ~ 80%, Ti85 ~ 95% in flyash in above-mentioned second method。
Fused salt electrolysis process electrolysis is adopted to contain SiO2、Al2O3、Fe2O3、TiO2、MgO、CaO、K2In the process of the flyash of the mixed oxides such as O, MgO, K2O and CaO and the AlF in cryolite3Reaction generates corresponding Al2O3And MgF2、Al2O3With KF, CaF2, MgF2, KF and CaF2Being the additive of aluminium electrolysis process, magnesium ion, potassium ion and calcium ion will not reduce precipitation。SiO2、Al2O3、Fe2O3、TiO2Acieral is obtained at cathode electrodeposition；Adopt aluminum liquid as negative electrode, on negative electrode aluminum liquid with electrolyte interface, SiO can occur simultaneously2、Fe2O3And TiO2Thermite reaction, generate aluminium oxide and acieral, and the aluminium oxide wherein generated obtain aluminum at cathode electrodeposition, adds the recovery rate of metal。
The fused salt electrolysis process of metal mixing oxide can be directly produced alloy from the mixture of metal-oxide, is a kind of new electrolysis process；The present invention passes through fused salt electrolysis process treated coal ash, and alloy is prepared in the direct electro-deposition of oxide such as aluminum, silicon, titanium and ferrum, it is achieved the green high-efficient comprehensive utilization of flyash, there is technique simple, can produce at existing industrial aluminum electrolysis bath, and flow process is short, the advantage that can be continuously produced。
Accompanying drawing explanation
Fig. 1 is the electrolytic cell assembly structural representation in the embodiment of the present invention 1；
Fig. 2 is the electrolytic cell assembly structural representation in the embodiment of the present invention 6；
In figure, 1, iron crucible, 2, small-sized anode rod, 3, resistance furnace, 4, graphite crucible (small electrolytic groove), 5, corundum liner, 6, small-sized anode, 7, ice crystal ground mass fused salt, 8, aluminum liquid (negative electrode), 9, hopper, 10, anode bus beam, 11, anode electrolytic cell guide rod, 12, pot shell, 13, anode electrolytic cell, 14, ice crystal ground mass molten salt electrolyte, 15, electrolysis bath aluminum liquid (negative electrode), 16, carbon lining, 17, cathode steel bar, 18, heat-insulation layer。
Detailed description of the invention
The fine coal ash composition selected in the embodiment of the present invention is by weight percentage containing Al2O339.04 ~ 52.80%, SiO234.30 ~ 55.24%, CaO0.25 ~ 3.90%, TiO20.77 ~ 1.97%, Fe2O31.50 ~ 6.20%, MgO0.10 ~ 3.70%, K2O0.01 ~ 2.10%, surplus is impurity。
The aluminium oxide selected in the embodiment of the present invention is commercial alumina, purity by weight 98.60 ~ 99.66%。
Cryolite (the Na selected in the embodiment of the present invention3AlF6) it is industry cryolite, purity by weight >=99%。
The AlF selected in the embodiment of the present invention3For commercial industrial products, purity by weight >=99%。
In the embodiment of the present invention, the current efficiency of electrolytic process is 40 ~ 60%。
Metal base aluminium electrolytic inert anode in the embodiment of the present invention is metal base aluminium electrolytic inert anode disclosed in patent CN1203217C, the composition of the metal base aluminium electrolytic inert anode selected is 40 ~ 100% containing Fe, Ni, Cr and Cu by weight percentage, is 0 ~ 60% containing Ag and Zn。
The carbon anode adopted in the embodiment of the present invention is industrial electrolysis aluminium anode carbon block。
Embodiment 1
By Na3AlF6And AlF3Mix homogeneously makes ice crystal ground mass fused salt, and mixed proportion presses NaF and the AlF in ice crystal ground mass fused salt3Mol ratio be 2；
Metallic aluminium is placed in electrolysis bath；Being placed in electrolysis bath by ice crystal ground mass fused salt again, be subsequently adding flyash, the addition of flyash is the 5% of ice crystal ground mass fused salt and flyash gross weight；Fine coal ash composition is by weight percentage containing Al2O352.75%, SiO238.05%, CaO3.88%, TiO21.97%, Fe2O31.86%, MgO0.51%, K2O0.10%, surplus is impurity；
Heating ice crystal ground mass fused salt and flyash to 910 DEG C, metallic aluminium is melted into aluminum liquid, and aluminum liquid, as negative electrode, adopts carbon anode as anode；Energising carries out electrolysis, and the electric current density controlled between negative electrode and anode is 0.4A/cm2, electrolysis time is 8h, and when starting after electrolysis, per half an hour adds a flyash in electrolysis bath, when the fine coal ash quantity every time added is start electrolysis in electrolysis bath the 20% of flyash gross weight；Electrolysis complete after on negative electrode formation of deposits acieral；Electrolytic cell assembly structure is as shown in Figure 1；
The composition of acieral is by weight percentage containing Al71.9%, Si19.0%, Fe6.5%, Ti2.1%, and surplus is impurity；The response rate of metal respectively Al70%, Si90%, Fe80%, Ti95% in flyash。
Embodiment 2
Fused salt electrolysis process extracts the method for metal with embodiment 1 from flyash, and difference is in that:
(1) NaF and the AlF in ice crystal ground mass fused salt3Mol ratio be 2.2；
(2) in electrolysis bath, the addition of flyash is the 3% of ice crystal ground mass fused salt and flyash gross weight；Fine coal ash composition is by weight percentage containing Al2O339.04%, SiO255.24%, CaO0.25%, TiO20.77%, Fe2O33.76%, MgO0.10%, K2O0.01%, surplus is impurity；
(3) heating ice crystal ground mass fused salt and flyash to 955 DEG C, adopt inert anode as anode, described inert anode is metal base aluminium electrolytic inert anode；Energising carries out electrolysis, and the electric current density between negative electrode and anode is 0.6A/cm2, electrolysis time is 7h；The fine coal ash quantity every time added be start electrolysis time electrolysis bath in flyash gross weight 30%；
(4) composition of acieral is by weight percentage containing Al74.6%, Si19.7%, Fe2.8%, Ti2.3%, and surplus is impurity；The response rate of metal respectively Al80%, Si85%, Fe70%, Ti90% in flyash。
Embodiment 3
Fused salt electrolysis process extracts the method for metal with embodiment 1 from flyash, and difference is in that:
(1) NaF and the AlF in ice crystal ground mass fused salt3Mol ratio be 2.4；
(2) in electrolysis bath, the addition of flyash is the 10% of ice crystal ground mass fused salt and flyash gross weight；Fine coal ash composition is by weight percentage containing Al2O347.11%, SiO234.30%, CaO3.90%, TiO21.86%, Fe2O36.20%, MgO3.70%, K2O2.10%, surplus is impurity；
(3) ice crystal ground mass fused salt and flyash are heated to 965 DEG C；Energising carries out electrolysis, and the electric current density between negative electrode and anode is 0.7A/cm2, electrolysis time is 6h；The fine coal ash quantity every time added be start electrolysis time electrolysis bath in flyash gross weight 40%；
(4) composition of acieral is by weight percentage containing Al67.9%, Si17.9%, Fe5.4%, Ti8.4%, and surplus is impurity；The response rate of metal respectively Al60%, Si70%, Fe60%, Ti85% in flyash。
Embodiment 4
Fused salt electrolysis process extracts the method for metal with embodiment 1 from flyash, and difference is in that:
(1) NaF and the AlF in ice crystal ground mass fused salt3Mol ratio be 2.6；
(2) in electrolysis bath, the addition of flyash is the 8% of ice crystal ground mass fused salt and flyash gross weight；Fine coal ash composition is by weight percentage containing Al2O349.63%, SiO240.27%, CaO2.96%, TiO21.25%, Fe2O31.50%, MgO2.21%, K2O1.63%, surplus is impurity；
(3) heating ice crystal ground mass fused salt and flyash to 975 DEG C, adopt inert anode as anode, described inert anode is metal base aluminium electrolytic inert anode；Energising carries out electrolysis, and the electric current density between negative electrode and anode is 0.8A/cm2, electrolysis time is 5h；The fine coal ash quantity every time added be start electrolysis time electrolysis bath in flyash gross weight 60%；
(4) composition of acieral is by weight percentage containing Al75.3%, Si17.9%, Fe2.8%, Ti3.2%, and surplus is impurity；The response rate of metal respectively Al50%, Si70%, Fe60%, Ti85% in flyash。
Embodiment 5
Fused salt electrolysis process extracts the method for metal with embodiment 1 from flyash, and difference is in that:
(1) NaF and the AlF in ice crystal ground mass fused salt3Mol ratio be 2.8；
(2) in electrolysis bath, the addition of flyash is the 5% of ice crystal ground mass fused salt and flyash gross weight；Fine coal ash composition is by weight percentage containing Al2O340.53%, SiO250.14%, CaO3.32%, TiO21.65%, Fe2O32.39%, MgO0.88%, K2O0.56%, surplus is impurity；
(3) ice crystal ground mass fused salt and flyash are heated to 985 DEG C；Energising carries out electrolysis, and the electric current density between negative electrode and anode is 1.2A/cm2, electrolysis time is 3h；The fine coal ash quantity every time added be start electrolysis time electrolysis bath in flyash gross weight 80%；
(4) composition of acieral is by weight percentage containing Al75.9%, Si19.8%, Fe2.5%, Ti1.3%, and surplus is impurity；The response rate of metal respectively Al75%, Si85%, Fe75%, Ti90% in flyash。
Embodiment 6
By Na3AlF6And AlF3Mix homogeneously makes ice crystal ground mass fused salt, and mixed proportion presses NaF and the AlF in ice crystal ground mass fused salt3Mol ratio be 2；
Metallic aluminium is placed in electrolysis bath；Being placed in electrolysis bath by ice crystal ground mass fused salt again, be subsequently adding the mixed material of flyash and aluminium oxide, in mixed material, flyash accounts for the 10% of mixed material gross weight, and all the other are aluminium oxide, and mixed material accounts for the 5% of ice crystal ground mass fused salt and mixed material gross weight；Fine coal ash composition is with embodiment 1；
Heating ice crystal ground mass fused salt and mixed material to 930 DEG C, metallic aluminium fusing forms aluminum liquid as negative electrode；Adopt carbon anode as anode；
Energising carries out electrolysis, and the electric current density controlled between negative electrode and anode is 0.4A/cm2, electrolysis time is 8h, and after starting electrolysis, per half an hour adds the mixed material of a flyash and aluminium oxide in electrolysis bath, and in mixed material, flyash accounts for the 10% of mixed material gross weight；The mixture doses every time added be start electrolysis time electrolysis bath in mixed material gross weight 20%；Electrolysis complete after on negative electrode formation of deposits acieral；Electrolytic cell assembly structure is as shown in Figure 2；
The composition of acieral is by weight percentage containing Al95.8%, Si2.9%, Fe0.8%, Ti0.3%, and surplus is impurity；The response rate of metal respectively Al80%, Si90%, Fe80%, Ti95% in flyash。
Embodiment 7
Fused salt electrolysis process extracts the method for metal with embodiment 6 from flyash, and difference is in that:
(1) NaF and the AlF in ice crystal ground mass fused salt3Mol ratio be 2.2；
(2) in mixed material, flyash accounts for the 20% of mixed material gross weight, and all the other are aluminium oxide, and mixed material accounts for the 6% of ice crystal ground mass fused salt and mixed material gross weight；Fine coal ash composition is with embodiment 2；
(3) heating ice crystal ground mass fused salt and mixed material to 955 DEG C, the electric current density between negative electrode and anode is 0.6A/cm2, electrolysis time is 7h, and in mixed material, flyash accounts for the 20% of mixed material gross weight；The mixture doses every time added be start electrolysis time electrolysis bath in mixed material gross weight 30%；
(4) composition of acieral is by weight percentage containing Al92.8%, Si5.6%, Fe0.9%, Ti0.5%, and surplus is impurity；The response rate of metal respectively Al70%, Si80%, Fe70%, Ti90% in flyash。
Embodiment 8
Fused salt electrolysis process extracts the method for metal with embodiment 6 from flyash, and difference is in that:
(1) NaF and the AlF in ice crystal ground mass fused salt3Mol ratio be 2.4；
(2) in mixed material, flyash accounts for the 30% of mixed material gross weight, and all the other are aluminium oxide, and mixed material accounts for the 4% of ice crystal ground mass fused salt and mixed material gross weight；Fine coal ash composition is with embodiment 3；
(3) heating ice crystal ground mass fused salt and mixed material to 965 DEG C, the electric current density between negative electrode and anode is 0.7A/cm2, electrolysis time is 6h, and in mixed material, flyash accounts for the 30% of mixed material gross weight；The mixture doses every time added be start electrolysis time electrolysis bath in mixed material gross weight 40%；
(4) composition of acieral is by weight percentage containing Al90.7%, Si5.3%, Fe1.3%, Ti2.5%, and surplus is impurity；The response rate of metal respectively Al60%, Si80%, Fe75%, Ti85% in flyash。
Embodiment 9
Fused salt electrolysis process extracts the method for metal with embodiment 6 from flyash, and difference is in that:
(1) NaF and the AlF in ice crystal ground mass fused salt3Mol ratio be 2.6；
(2) in mixed material, flyash accounts for the 40% of mixed material gross weight, and all the other are aluminium oxide, and mixed material accounts for the 2% of ice crystal ground mass fused salt and mixed material gross weight；Fine coal ash composition is with embodiment 4；
(3) heating ice crystal ground mass fused salt and mixed material to 975 DEG C, the electric current density between negative electrode and anode is 0.8A/cm2, electrolysis time is 5h, and in mixed material, flyash accounts for the 40% of mixed material gross weight；The mixture doses every time added be start electrolysis time electrolysis bath in mixed material gross weight 60%；
(4) composition of acieral is by weight percentage containing Al90.3%, Si6.8%, Fe1.2%, Ti1.5%, and surplus is impurity；The response rate of metal respectively Al50%, Si70%, Fe60%, Ti85% in flyash。
Embodiment 10
Fused salt electrolysis process extracts the method for metal with embodiment 6 from flyash, and difference is in that:
(1) NaF and the AlF in ice crystal ground mass fused salt3Mol ratio be 2.8；
(2) in mixed material, flyash accounts for the 60% of mixed material gross weight, and all the other are aluminium oxide, and mixed material accounts for the 8% of ice crystal ground mass fused salt and mixed material gross weight；Fine coal ash composition is with embodiment 5；
(3) heating ice crystal ground mass fused salt and mixed material to 985 DEG C, the electric current density between negative electrode and anode is 1.0A/cm2, electrolysis time is 3h, and in mixed material, flyash accounts for the 60% of mixed material gross weight；The mixture doses every time added be start electrolysis time electrolysis bath in mixed material gross weight 80%；
(4) composition of acieral is by weight percentage containing Al85.2%, Si12.3%, Fe1.6%, Ti0.8%, and surplus is impurity；The response rate of metal respectively Al50%, Si80%, Fe80%, Ti95% in flyash。
Claims (3)
1. the method that a fused salt electrolysis process extracts metal from flyash, it is characterised in that sequentially include the following steps:
(1) by Na3AlF6And AlF3Mix homogeneously makes ice crystal ground mass fused salt, and mixed proportion presses NaF and the AlF in ice crystal ground mass fused salt3Mol ratio be 2 ~ 2.8；
(2) ice crystal ground mass fused salt is placed in electrolysis bath, it is subsequently adding the mixed material of flyash and aluminium oxide, in mixed material, flyash accounts for the 10 ~ 60% of mixed material gross weight, and all the other are aluminium oxide, and mixed material accounts for the 2 ~ 8% of ice crystal ground mass fused salt and mixed material gross weight；
(3) heating ice crystal ground mass fused salt and mixed material to 930 ~ 985 DEG C, be then electrified to carry out electrolysis, the electric current density controlled between negative electrode and anode is 0.4 ~ 1.0A/cm2, electrolysis time is 3 ~ 8h, electrolysis complete after on negative electrode formation of deposits acieral；On negative electrode, the composition of the acieral of deposition is by weight percentage containing Al85 ~ 96%, Si2.5 ~ 12.5%, Fe0.8 ~ 1.6%, Ti0.3 ~ 2.5%, and surplus is impurity。
2. the method that a kind of fused salt electrolysis process according to claim 1 extracts metal from flyash, it is characterized in that after starting electrolysis, per half an hour adds the mixed material of a flyash and aluminium oxide in electrolysis bath, and in mixed material, flyash accounts for the 10 ~ 60% of mixed material gross weight；The mixture doses every time added be start electrolysis time electrolysis bath in mixed material gross weight 20 ~ 80%。
3. the method that a kind of fused salt electrolysis process according to claim 1 extracts metal from flyash, it is characterised in that the negative electrode adopted during electrolysis is aluminum liquid, and anode is carbon anode。
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