CN1443877A - Metal base aluminium electrolytic inert anode and its preparation method - Google Patents
Metal base aluminium electrolytic inert anode and its preparation method Download PDFInfo
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Abstract
The present invention relates to an inert anode (also called nonexpendable anode) material used in electrolysis industry of aluminium, magnesium and rare eartly, etc. When said material is used as anode to make aluminium electrolysis, the oxygen gas can be separated out from the anode surface. In the electrolytic experimentation said anode shows the good resistance to oxidation and resistance to cryolire fused salt corrosion, and its aluminium product quality can be up to above 98%, and said anode material is made up by selecting and using two-component or multicomponent alloy of the metals of Cr, Ni, Fe, Co, Ti, Cu, Al and Mn. Said invention adopts the smelting or powder metallurgy process to prepare anode, and said anode is good in electric conductivity and thermal conductivity.
Description
The technical field is as follows: the invention relates to the field of molten salt electrolysis in nonferrous metallurgy, and mainly develops an electrolytic industrial metal anode material such as aluminum, magnesium, rare earth and the like and a preparation method thereof.
Secondly, background art: hall used in aluminum electrolysis industry at presentThe erlu method, the anodes are all carbon anodes (also called graphite anodes). The reason why the metal-based anode cannot be used in the past is that the problem of contamination of the product due to the participation of the metal-based anode in the electrolytic reaction cannot be solved. Graphite is used as an anode, anode carbon is oxidized and consumed during electrolysis, a large amount of greenhouse gases are discharged, and electrode reaction is as follows: (ii) a And then, carrying out secondary reaction on the anode gas: more anode carbon is consumed and a large amount of toxic CO gas is generated. Theoretically, 333 kilograms of carbon is consumed for each ton of aluminum produced, and the actual consumption of aluminum plants is about 450-600 kilograms, so that the consumption of high-quality carbon materials is larger and larger, the price is increased, and the anode cost accounts for about 14-22% of the aluminum production cost.
The existing consumable carbon anode has the following defects:
1. a large amount of high-quality coke and petroleum coke are consumed;
2. discharge large amount of greenhouse gases and toxic gases, such as CF4、CF6PNAH polycyclic aromatic hydrocarbon (generated in the anode production process), Volatile Organic Compounds (VOC), HF and SOxCOS and NOx；
3. The anode replacement cost is high and the labor intensity is high;
4. the unit capacity is huge in one-time investment.
Thirdly, the invention content:
1. the purpose of the invention is as follows: the invention provides a metal-based aluminum electrolysis inert anode and a preparation method thereof, aiming at solving the defects caused by taking graphite as an anode and the problems in the aspect of product pollution caused by taking metal as the anode to participate in an electrolysis reaction.
2. The technical scheme is as follows: the invention is realized by the following technical scheme:
a metal-based aluminum electrolysis inert anode is applied to molten salt electrolysis of aluminum, magnesium and rare earth as an anode, and is characterized in that: the anode is formed by binary alloy or multi-element alloy with the following metal elements: nickel, iron, cobalt, chromium, titanium, copper, aluminum, silver, zinc, manganese, iridium, platinum, hafnium, tantalum, niobium, tungsten, molybdenum, yttrium, zirconium, vanadium, lanthanide elements.
The anode alloy material is AxByWherein x is the mass percent of A, y is the mass percent of B, x is 40-100%, and y is 0-60%; a is composed of one or more elements of iron, nickel, cobalt, chromium, titanium, copper and aluminum, and B is composed of one or more elements of silver, zinc, manganese, iridium, platinum, hafnium, tantalum, niobium, tungsten, molybdenum, yttrium, zirconium, vanadium, lanthanide metal elements, boron and carbon nonmetal elements.
Anode material composition AxByWherein x is the mass percent of A, y is the mass percent of B, x is 90-100%, and y is 0-10%; a is composed of one or more elements of iron, nickel, cobalt, chromium, titanium, copper and aluminum, and B is composed of one or more elements of silver, zinc, manganese, iridium, platinum, hafnium, tantalum, niobium, tungsten, molybdenum, yttrium, zirconium, vanadium, lanthanide metal elements, boron and carbon nonmetal elements.
An oxide protective film is formed on the surface of the metal anode.
The preparation method of the metal-based aluminum electrolysis inert anode material is characterized by comprising the following steps: the preparation method comprises two preparation methods:
a. an alloy smelting method comprises the following steps: the anode material provided by claim 1 is selected and made of a material which can be selected, and after the anode is made by a conventional alloy smelting method, the made anode is pre-oxidized at high temperature before use, so that an oxide protective film is formed on the surface of the metal anode.
b. Powder metallurgy: the method comprises the following four steps of material preparation, material mixing, molding and sintering:
(1) preparing materials: ball milling the single metal powder of claim 1 for 48 hr to obtain 200 mesh powder with the ratio of ball to material to alcohol being 4 to 1 to 1.5; then mixing various metal powders or metal powders and boron and carbon nonmetal powders, and ball milling for 5 hours to fully and uniformly mix the powders.
(2) Mixing materials: after drying, water or polyvinyl alcohol is used as a binder to be evenly mixed, and the mixture is placed for 2 to 10 hours.
(3) Molding: cold pressing at normal temperature of 400 plus 800 MPa.
(4) And (3) sintering: and naturally drying the cold-pressed sample at normal temperature, sintering the cold-pressed sample in an inert atmosphere silicon-molybdenum furnace within the sintering temperature range for 4-8 hours, and cooling the cold-pressed sample to room temperature along with the furnace temperature under the protection of the inert atmosphere to obtain the metal-based aluminum electrolysis inert anode finished product.
The anode prepared after sintering is pre-oxidized at high temperature before use, so that an oxide protective film is formed on the surface of the metal anode.
3. The advantages and effects are as follows: the advantages of the invention can not only solve the above problems, but also have the following advantages:
(1) and byproduct O while realizing green production2Economic benefits can be generated;
(2) and the cell voltage can be greatly reduced by matching with the wettable cathode, so that the energy-saving effect is realized.
The scope of current research includes primarily oxide anodes, nickel ferrite cermet anodes, and metal anodes. The oxide anode is mainly SnO2、ZrO2And the cermet is studied to be composed of a Ni-Fe-O ceramic phase and a metal phase composed of Cu, Ni, Ag and the like. Metal anodes have been studied only rarely. The metal anode has better conductivity and thermal shock resistance than oxide ceramic and metal ceramic anodes, can obviously reduce the voltage drop of the anode and the service life of the anode in use, and has low cost. The research aims to develop a metal anode to replace the consumable carbon anode used at present, realize the huge benefits of energy conservation, environmental protection and unit productivity investment, and promote the rapid development of the aluminum electrolysis industry. The mechanism of the metal anode work (electrolysis) isthat the nascent oxygen (mainly high-activity monatomic oxygen) precipitated on the surface of the anode oxidizes the anode matrix,the corresponding metal oxide composite film is generated, and the film can not only prevent the metal anode substrate from further oxidation, but also conduct electricity.
Fourthly, the specific implementation mode:
the invention is based on the focus and hot spot of the aluminum industry development in the world at present, and the high-temperature alloy aluminum which is successfully developed on the basis of a large amount of experimental researchesAnd electrolyzing the inert anode material. A metal anode material according to AxByThe composition is characterized in that x is the mass percentage of A, y is the mass percentage of B, the value of x is 40-100%, and the value of y is 0-60%. Wherein A is composed of single or multiple elements of iron (Fe), nickel (Ni), cobalt (Co), chromium (Cr), copper (Cu), titanium (Ti) and aluminum (Al), and B is composed of single or multiple elements of silver (Ag), zinc (Zn), manganese (Mn), iridium (Ir), platinum (Pt), hafnium (Hf), tantalum (Ta), niobium (Nb), tungsten (W), molybdenum (Mo), yttrium (Y), zirconium (Zr), vanadium (V), lanthanide metal elements, boron (B) and carbon (C).
The anode material development is realized by the following steps and ways:
the anode material can be selected from the materials, the alloy is produced by adopting a smelting, powder metallurgy or mechanical alloying method, and then the anode with a certain shape is processed. The smelting method adopts different smelting systems according to different selected alloy materials. When the powder metallurgy method is adopted, different preparation processes are selected according to different materials during sample pressing and sintering.
The anti-oxidation and anti-corrosion high-temperature alloy component is added based on the corrosion resistance of the high-temperature alloy, so that the prepared anode material has excellent conductivity, is convenient to connect with a power supply, has wide material source, is low in price and low in manufacturing cost, and is beneficial to industrial large-scale use.
The anode material is prepared by a conventional alloy smelting method, and the anode material is required to be produced under the conditions of high temperature and high vacuum. The powder metallurgy preparation method comprises four steps of material preparation, material mixing, molding and sintering.
(1) Preparing materials: ball milling single metal powder for 48 hr to obtain powder of 200 mesh size, the ratio of ball to material to alcohol being 4 to 1 to 1.5; then, various metal powders are mixed and ball-milled for 5 hours to be fully and uniformly mixed.
(2) Mixing materials: after drying, water or polyvinyl alcohol is used as a binder to be evenly mixed, and the mixture is placed for 2 hours.
(3) And forming: cold pressing at normal temperature 500 MPa.
(4) And sintering: and naturally drying the cold-pressed sample at normal temperature, sintering the cold-pressed sample in a silicon-molybdenum furnace in an inert atmosphere within a sintering temperature range for 4-8 hours, and then cooling the cold-pressed sample to room temperature along with the furnace temperature under the protection of the inert atmosphere.
Example one:
taking the following components in percentage by mass: the anode is prepared from 37% of cobalt (Co), 18% of copper (Cu), 19% of nickel (Ni), 23% of iron (Fe) and 3% of silver (Ag) by a powder metallurgy method, and is pre-oxidized at 1000 ℃ before use to form an oxide protective film on the surface of the metal anode. At 850 deg.C, the anode current density is 1.0A/cm2NaF and AlF3Has a molar ratio of 1.8 and an alumina concentration (mass percentage content) of 4.0 percent and has a composition of NaF-AlF3-NaCl-CaF2-Al2O3Has been used for electrolysis for up to several 40 hours. During electrolysis, high-purity graphite is used as a cathode, and a graphite crucible with corundum lining is vertically inserted into the cathode and the anode, wherein the polar distance is 3.0 cm. The application result shows that the electrolysis process is stable, the cell pressure is 4.1-4.5 volts, the anode corrosion rate in the aluminum electrolysis process is low, and the quality of the aluminum product reaches 98.35%. Solves the problem of product pollution caused by alloy components in the process of metal-based inert anode electrolysis.
The overall electrode reaction of the electrolytic process can be written as:
during electrolysis, a large amount of gas is generated around the anode, and oxygen (O) is released according to the structural components of the anode and the composition of the electrolyte2)。
Example two:
taking the following components in percentage by mass: 22% of chromium (Cr), 35% of iron (Fe), 10% of copper (Cu), 24% of nickel (Ni), 8% of aluminum powder (Al) and 1% of tungsten powder (W). And preparing the anode by a powder metallurgy method. The experiment was performed under the same conditions as in example one. Test results show that the electrolysis process is stable, the cell pressure is 3.9-4.6 volts, the anodic corrosion rate in the aluminum electrolysis process is low, and the qualityof aluminum products reaches 98.34%.
Example three:
taking the following components in percentage by mass: 47% of nickel (Ni), 14% of chromium (Cr), 26% of iron (Fe), 11% of copper (Cu) and 2% of zinc (Zn). The anode is prepared by adopting a high-temperature smelting method. The electrolysis test was carried out under the same conditions as in example one. The electrolysis process is stable, the cell pressure is 4.1-4.3 volts, the anode corrosion rate in the aluminum electrolysis process is low, and the quality of an aluminum product reaches 99.01 percent.
Example four:
taking the mass percentage as follows; 47% of nickel (Ni), 52% of iron (Fe) and 1% of zinc (Zn), which are prepared by a powder metallurgy method, and are pre-oxidized at 1100 ℃ before use to form a protective film on the surface of a metal anode; anode current density 1.0A/cm at 940 deg.C2NaF and AlF3The molar ratio of (A) is 2.4, the concentration of alumina (mass percentage content) is 5.0 percent, and the composition is NaF-AlF3-CAF2-AL2O3The electrolyte is electrolyzed for 80 hours, the electrolysis process is stable, the cell voltage is 4.2-4.7 volts, the anode corrosion speed in the aluminum electrolysis process is low, and the quality of an aluminum product is 98.11%.
Claims (6)
1. A metal-based aluminum electrolysis inert anode is applied to molten salt electrolysis of aluminum, magnesium and rare earth as an anode, and is characterized in that: the anode is formed by binary alloy or multi-element alloy with the following metal elements: nickel, iron, cobalt, chromium, titanium, copper, aluminum, silver, zinc, manganese, iridium, platinum, hafnium, tantalum, niobium, tungsten, molybdenum, yttrium, zirconium, vanadium, lanthanide elements.
2. The metal-based aluminum electrolysis inert anode of claim 1, wherein: the anode alloy material is AxByWherein x is the mass percent of A, y is the mass percent of B, x is 40-100%, and y is 0-60%; a is composed of one or more elements of iron, nickel, cobalt, chromium, titanium, copper and aluminum, and B is composed of one or more elements of silver, zinc, manganese, iridium, platinum, hafnium, tantalum, niobium, tungsten, molybdenum, yttrium, zirconium, vanadium, lanthanide metal elements, boron and carbon nonmetal elements.
3. The metal-based aluminum electrolysis inert anode of claim 1, wherein: anode material composition AxByWherein x is the mass percent of A, y is the mass percent of B, x is 90-100%, and y is 0-10%;a is composed of one or more elements of iron, nickel, cobalt, chromium, titanium, copper and aluminum, and B is composed of one or more elements of silver, zinc, manganese, iridium, platinum, hafnium, tantalum, niobium, tungsten, molybdenum, yttrium, zirconium, vanadium, lanthanide metal elements, boron and carbon nonmetal elements.
4. The metal-based aluminum electrolysis inert anode of claim 1, wherein: an oxide protective film is formed on the surface of the metal anode.
5. The method for preparing the metal-based aluminum electrolysis inert anode material according to claim 1, wherein the method comprises the following steps: the preparation method comprises two preparation methods:
a. an alloy smelting method comprises the following steps: the anode material provided by claim 1 is selected and made of a material which can be selected, and after the anodeis made by a conventional alloy smelting method, the made anode is pre-oxidized at high temperature before use, so that an oxide protective film is formed on the surface of the metal anode.
b. Powder metallurgy: the method comprises the following four steps of material preparation, material mixing, molding and sintering:
(1) preparing materials: ball milling the single metal powder of claim 1 for 48 hr to obtain 200 mesh powder with the ratio of ball to material to alcohol being 4 to 1 to 1.5; then mixing various metal powders or metal powders and boron and carbon nonmetal powders, and ball milling for 5 hours to fully and uniformly mix the powders.
(2) Mixing materials: after drying, water or polyvinyl alcohol is used as a binder to be evenly mixed, and the mixture is placed for 2 to 10 hours.
(3) Molding: cold pressing at normal temperature of 400 plus 800 MPa.
(4) And (3) sintering: and naturally drying the cold-pressed sample at normal temperature, sintering the cold-pressed sample in an inert atmosphere silicon-molybdenum furnace within the sintering temperature range for 4-8 hours, and cooling the cold-pressed sample to room temperature along with the furnace temperature under the protection of the inert atmosphere to obtain the metal-based aluminum electrolysis inert anode finished product.
6. The method for preparing the metal-based aluminum electrolysis inert anode material according to claim 5, wherein the method comprises the following steps: the anode prepared after sintering is pre-oxidized at high temperature before use, so that an oxide protective film is formed on the surface of the metal anode.
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