CN104532300B - A kind of method of electrolytic preparation alusil alloy - Google Patents
A kind of method of electrolytic preparation alusil alloy Download PDFInfo
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- CN104532300B CN104532300B CN201410830210.3A CN201410830210A CN104532300B CN 104532300 B CN104532300 B CN 104532300B CN 201410830210 A CN201410830210 A CN 201410830210A CN 104532300 B CN104532300 B CN 104532300B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/36—Alloys obtained by cathodic reduction of all their ions
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/02—Electrodes; Connections thereof
- C25C7/025—Electrodes; Connections thereof used in cells for the electrolysis of melts
Abstract
A kind of method of electrolytic preparation alusil alloy, during electrolytic preparation alusil alloy, uses the carbon anode prepared at interior raw material by coal as the silicon source in alusil alloy；It is that coal is reacted with hydrochloric acid solution, after solid-liquid separation, obtains siliceous Filter Tuber For Clean Coal, prepared by calcining again and forge rear coal, carry out mixing joining with after-smithing petroleum coke, add coal tar pitch kneading, after molding and roasting, preparing the carbon anode of certain silicone content, this anode can be used for electrolytic preparation alusil alloy；Acidleach filtrate is evaporated, obtains solid chloride and hydrogen chloride gas, collect the hydrogen chloride gas circulating leaching for hydrochloric acid.Sufficient raw of the present invention, the comprehensive utilization value of coal is high, has technological process short, and production cost is low, and level of residue is little, and hydrochloric acid such as can recycle at the feature, and preparing Novel carbon anode for coal provides processing technology routine, has broad application prospects.
Description
Technical field
A kind of method that the present invention relates to electrolytic preparation alusil alloy.
Background technology
Alusil alloy is extensively applied molten with transportation, electric power, automobile and aeronautical light field, current commonly used fine aluminium and pure silicon
Joining method and produce alusil alloy, alloy production link is many, and the cycle is long, and energy consumption is high, and scale of investment is big.
China is the country that petroleum resources are in short supply, and the petroleum import dependency degree of China has reached about 50%-60% in recent years, and
Along with the anxiety of petroleum resources, the petroleum coke of one of carbon anode raw material relying on Petroleum Production also becomes in short supply.
China has quite abundant coal reserves, also the cheapest more than petroleum coke, uses coal to prepare aluminum carbon anode
Obviously advantage is had in terms of cost of material.But, owing to aluminum carbon anode has strict requirements to ash, and coal
In usually contain higher ash, accordingly, it would be desirable to coal is carried out deliming process.At present, utilize acid-base method, hydrogen fluoride,
Although the ash in coal can be reduced to less than 1% by the technology such as solvent extraction and oil briquetting floating method, but these de-ash process have
Long flow path and high in cost of production shortcoming.
Patent CN1376813A discloses the method for one " with aluminium, silicon and titanium multielement alloy produced by electrolytic process ", by aluminium oxide,
The oxide such as silicon oxide and titanium oxide adds electrolysis bath Direct Electrolysis to and produces aluminium, silicon and titanium multielement alloy, but silicon and titanium are in aluminum liquid
Segregation is serious, and current efficiency is low, and normal production of electrolysis bath is also resulted in the biggest difficulty.
Patent CN101255572A discloses " a kind of method utilizing calcined anthracite to prepare aluminum carbon anode ", selects ash little
Low ash anthracite in 5% is calcined, and then mixes and joins after-smithing petroleum coke and prepare aluminum carbon anode.Owing to this anthracite is not carried out
Deliming processes, and ash is the highest, so the ratio of petroleum replacing Jiao is relatively low, additionally, the anthracitic reserves of low ash do not enrich,
The source of raw material is the most limited.
Patent CN101225530A discloses " low-ash carbonaceous raw material application in preparing prebaked anode " method, selects low
Carbon residue after ash anthracite, bituminous coal, bamboo charcoal, Linesless charcoal, waste plastics or scrap rubber carbonization as producing the auxiliary material of prebaked anode,
Patent requirements above-mentioned carbon residue content of ashes is less than 2.8%, under this content of ashes requires, it is clear that can improve mixing of carbonaceous raw material
Proportioning example, but corresponding low-ash carbonaceous raw material source is more rare.
Patent CN101698947A discloses " preparation method of a kind of aluminium electrolysis carbon anode ", by flotation de-ash coal and powdery calculogenesis
Oil coke mixing is calcined, and prepares compound calcined coke, is used for replacing part or all of petroleum coke and makes aluminum carbon anode.Patent
Requiring that the washability of coal, less than 2.5%, is required the highest by the content of ashes of flotation de-ash coal, the most little a part of coal meets
Demand.
Therefore, current carbon anode used for aluminium electrolysis typically uses the less carbon material of ash to produce, with petroleum coke as aggregate,
Use coal tar pitch as binding agent, be prepared from.And relating to carbon anode in existing technique is all how to remove all of impurity,
And use what technique to reduce the ash treatment in raw material as far as possible.But for various reasons, the de-ash process deliming effect of employing
Rate variance, the workload of deliming is big.But constantly rise now with the external crude oil with poor quality of China's import and heavy crude proportion, cause
The supply of high-quality petroleum coke has a certain degree of decline, thus aggravates the in short supply of aluminum high-quality petroleum coke.
Summary of the invention
It is an object of the invention to provide the electrolysis system of a kind of carbon anode that can obtain on the basis of need not the dedusting process of complexity
The method of standby alusil alloy.
The technical scheme is that
During electrolytic preparation alusil alloy, use the carbon anode prepared at interior raw material by coal as alusil alloy
In silicon source, the preparation of described carbon anode comprises the technical steps that:
A. coal powder is broken to below 100 mesh, adds the hydrochloric acid that mass percent concentration is 10-37% and carry out at 120-220 DEG C
Acid-leaching reaction, acid-leaching reaction dissolution pressure is 0.3-3Mpa, through solid-liquid separation and washing after reaction completely, obtains clean coal and acid
Immersion；
B. the clean coal of step a gained is carried out coal after calcining is forged at 1200-2000 DEG C；
C. with siliceous rear coal and the after-smithing petroleum coke forged as aggregate, with coal pitch of agglomerant kneading, through molding and roasting, charcoal sun is prepared
Pole.
In described step a, coal feedstock includes having anthracite, bituminous coal and/or brown coal.
Hydrochloric acid is 0.5-5L/Kg with the addition ratio of coal.
The described acid-leaching reaction time is 0.5-5.0 hour.
Siliceous forging rear coal and join raw material as producing mixing of pre-baked carbon anode, it is mixed dosage and with after-smithing petroleum coke mass ratio is
5:95-50:50。
With coal pitch of agglomerant kneading process in described step c, the quality of binding agent accounts for the 13%-18% of anode paste gross weight.
In described step b., calcination time 1-3 hour.
Described d. step pickle liquor is evaporated crystallization, obtains solid-state chloride, collects the hydrogen chloride gas that evaporation process produces simultaneously
Body, after absorbing with water, returns to step a for acid-leaching reaction.
Being particularly preferably addition mass percent concentration in described step a in the present invention is the hydrochloric acid of 15-25%, 180-200 DEG C
Under carry out acid-leaching reaction, acid-leaching reaction dissolution pressure is 1.0-2.0Mpa, and the acid-leaching reaction time is 2-3 hour.
Coal feedstock anthracite, bituminous coal and/or brown coal etc. in step a of the present invention；In coal feedstock, dioxide-containing silica is
3%～50% is advisable.After being processed by the acid leaching process of the present invention, silicon is optionally retained in coal, and other impurity quilt
Remove.
The present invention selects coal all to can be selected for as raw material, the coal of almost all kinds, uses the method for direct acidleach to remove coal
In ash impurities, during acidleach use reactor 120-220 DEG C of leaching, a step deliming removal of impurity i.e. can reach 95% with
On, simplify de-ash process flow process, reduce production cost；Meanwhile, the present invention also by add hydrochloric acid PROCESS FOR TREATMENT, and
Having the control of related parameter, in can ensure that coal, the removing of other impurity element is simultaneously completely so that silicon composition is retained in de-ash coal
In, for this siliceous clean coal characteristic, after calcining, Substitute For Partial petroleum coke prepares pre-baked anode for aluminum, and Direct Electrolysis produces aluminum silicon
Alloy.The present invention has broken away from the restriction that in existing carbon anode alternative materials coal, content of ashes is high, but also in ash content of coal
Valuable constituent silicon comprehensively utilized, in de-ash coal, siliceous composition is no longer regarded as impurity, can increase replacement oil
Burnt ratio.Additionally, decrease follow-up fine aluminium and pure silicon melts the link of the standby alusil alloy of preparation.The present invention is realizing coal replacement
While part petroleum coke, utilize silicon composition intrinsic in coal, if this part element silicon is selectively retained in coal,
While alleviating the burden of deliming operation, reduce into product cost, and the carbon anode prepared by the method for the present invention is direct
Electrolysis production alusil alloy, for alusil alloy produces, effectively prevent current commonly used fine aluminium and pure silicon mix-melting method is raw
Producing alusil alloy, alloy production link is many, and the cycle is long, and energy consumption is high.It is simple that whole technique has method, the advantages such as flow process is short.
To sum up, the present invention prepares carbon anode, on the one hand, widened the scope of application of coal resources, can make the production of carbon anode
Cost is remarkably decreased, and expands the raw material availability of carbon industry；On the other hand, making and the aluminum silicon of carbon anode can be reduced simultaneously
The production cost of alloy；The carbon anode prepared by form of the present invention uses this de-ash coal Substitute For Partial petroleum coke to prepare carbon anode,
The prepared siliceous carbon anode of coal of mixing can be used to Direct Electrolysis and goes out alusil alloy, compared with original technique, eliminates intermediate link,
Energy-saving and cost-reducing purpose can be reached.Prepare Novel carbon anode for coal and provide processing technology routine, before there is wide application
Scape；There is good economic benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is the process chart preparing Electrolytic Al-Si Alloys carbon anode with acid de-ash coal for raw material；
Detailed description of the invention
It is described further with specific embodiment below in conjunction with the accompanying drawings, but the present invention is not therefore subject to any restriction.
Embodiment 1
Recording anthracite ash is 32.04%, and wherein dioxide-containing silica is 20%, and volatilization is divided into 4.97%, is pulverized by anthracite
To 100 mesh, being then placed in acid-resistant reacting kettle carrying out acid-leaching reaction with the hydrochloric acid that concentration is 20wt%, reaction temperature is 180
DEG C, reaction pressure 1.5MPa, response time 2h, product obtain after filtration washing dioxide-containing silica be 21.5% clear
Clean coal, after measured, in anthracite, the removal efficiency of other metal impurities reaches more than 95% in addition to silicon, and de-ash coal is through 1400 DEG C of high temperature
Calcining, carry out mixing to mix joining with the ratio of mash form with after-smithing petroleum coke 40:60 in mass ratio, by grain size distribution, kneading,
Molding and calcining process, prepare siliceous prebaked anode sample, and its true density is 1.95g/cm3, bulk density is 1.49g/cm3,
Resistivity is 62.36 μ Ω m, comprcssive strength 34.5MPa, and wherein dioxide-containing silica is 8.6%, closes for electrolytic preparation aluminum silicon
Gold；Electrolytic production silicon from aluminum-silicon alloy content is 2.0%.
Embodiment 2
Recording anthracite ash is 17.14%, and wherein dioxide-containing silica is 7.8%, and volatilization is divided into 4.42%,
Bituminous coal powder is broken to below 100 mesh, is then placed in acid-resistant reacting kettle carrying out acid-leaching reaction with the hydrochloric acid that concentration is 25wt%, reaction
Temperature is 200 DEG C, reaction pressure 2.0MPa, response time 2h, and product, after filtration washing, obtains silicon dioxide and contains
Amount is the clean coal of 8.6%, and de-ash coal is through 1500 DEG C of high-temperature calcinations, with mash form and after-smithing petroleum coke 20:80 in mass ratio
Ratio carry out mixing and mix and join, by grain size distribution, kneading, molding and calcining process, prepare siliceous prebaked anode sample, its
True density is 1.94g/cm3, bulk density is 1.49g/cm3, resistivity is 68.23 μ Ω m, and comprcssive strength is
35.3MPa, wherein dioxide-containing silica is 1.73%, for electrolytic preparation alusil alloy；Electrolytic production silicon from aluminum-silicon alloy contains
Amount is 0.40%.
Embodiment 3
Recording bituminous coal ash is 18.75%, and wherein dioxide-containing silica is 5.9%, and volatilization is divided into 22.28%, is broken to by coal dust
Below 100 mesh, being then placed in acid-resistant reacting kettle carrying out acid-leaching reaction with the hydrochloric acid that concentration is 37wt%, reaction temperature is 180
DEG C, reaction pressure 1.5MPa, response time 2.5h, product is after filtration washing, and obtaining dioxide-containing silica is 6.7%
Clean coal, de-ash coal, through 1500 DEG C of high-temperature calcinations, is carried out with the ratio of mash form with after-smithing petroleum coke 30:70 in mass ratio
Mixing is mixed and is joined, and by grain size distribution, kneading, molding and calcining process, prepares siliceous prebaked anode sample, and its true density is
1.91g/cm3, bulk density is 1.46g/cm3, resistivity is 75.86 μ Ω m, and comprcssive strength is 30.7MPa, wherein dioxy
SiClx content is 2.0%, for electrolytic preparation alusil alloy；After electrolysis, product silicon from aluminum-silicon alloy content is 0.47%.
Embodiment 4
Recording bituminous coal ash is 28.60%, and wherein dioxide-containing silica is 11.42%, and volatilization is divided into 17.75%, is broken to by coal dust
Below 200 mesh, being then placed in acid-resistant reacting kettle carrying out acid-leaching reaction with the hydrochloric acid that concentration is 37wt%, reaction temperature is 180
DEG C, reaction pressure 1.5MPa, response time 3h, product is after filtration washing, and obtaining dioxide-containing silica is 13.50%
Clean coal, de-ash coal, through 1400 DEG C of high-temperature calcinations, is carried out with the ratio of mash form with after-smithing petroleum coke 30:70 in mass ratio
Mixing is mixed and is joined, and by grain size distribution, kneading, molding and calcining process, prepares siliceous prebaked anode sample, and its true density is 1.89
g/cm3, bulk density is 1.44g/cm3, resistivity is 80.13 μ Ω m, and comprcssive strength is 30.2MPa, and wherein silicon dioxide contains
Amount is 4.0%, for electrolytic preparation alusil alloy；After electrolysis, product silicon from aluminum-silicon alloy content is 0.9%
Embodiment 5
Recording lignite ash and be divided into 12.64%, wherein dioxide-containing silica is 3.12%, and volatilization is divided into 43.75%, is broken to by coal dust
Below 200 mesh, being then placed in acid-resistant reacting kettle carrying out acid-leaching reaction with the hydrochloric acid that concentration is 10wt%, reaction temperature is 180
DEG C, reaction pressure 1.5MPa, response time 3.5h, product is after filtration washing, and obtaining dioxide-containing silica is 3.3%
Clean coal, de-ash coal, through 1500 DEG C of high-temperature calcinations, is carried out with the ratio of mash form with after-smithing petroleum coke 10:90 in mass ratio
Mixing is mixed and is joined, and by grain size distribution, kneading, molding and calcining process, prepares siliceous prebaked anode sample, and its true density is 1.97
g/cm3, bulk density is 1.50g/cm3, resistivity is 69 μ Ω m, and comprcssive strength is 31.6MPa, wherein dioxide-containing silica
It is 0.35%, for electrolytic preparation alusil alloy；After electrolysis, product silicon from aluminum-silicon alloy content is 0.1%.
Comparative example 1
Recording anthracite ash is 17.14%, and wherein dioxide-containing silica is 7.8%, and volatilization is divided into 4.42%, the granularity selection of coal
Being below 100 mesh, carry out acid-leaching reaction with the hydrochloric acid that concentration is 10wt% at ambient pressure, reaction temperature is 90 DEG C, the response time
4h, product is after filtration washing, and in coal, ash only has a small amount of removing, still contains the ash of 16.02%, wherein dioxy
SiClx content is 8.6%, and major impurity element is ferrum, calcium, magnesium and sodium etc..Pickling coal is through 1500 DEG C of high-temperature calcinations, with powder
Form carries out mixing to mix joining, by grain size distribution, kneading, molding and roasting with the ratio of after-smithing petroleum coke 20:80 in mass ratio
Operation, prepares prebaked anode sample, and its true density is 1.95g/cm3, bulk density is 1.49g/cm3, resistivity is
78.23 μ Ω m, comprcssive strength is 29.2MPa, and wherein dioxide-containing silica is 1.73%, when electrolytic experiment, due to anode
In containing too high impurity element, anode consumption substantially and has slag-off phenomenon (impurity element has catalytic action, causes anode volume
Outer consumption), electrolytic production does not contain only silicon, possibly together with the impurity such as ferrum, titanium.In coal, impurity element removing is not thorough, not only
Affect anode performance, and electrolytic process causes extra consumption, additionally, impurity pollutes negative electrode aluminum product in electrolytic process,
Increase follow-up remove impurity work.
Comparative example 2
Recording bituminous coal ash is 28.60%, and wherein dioxide-containing silica is 11.42%, and volatilization is divided into 17.75%, is broken to by coal dust
Below 200 mesh, being then placed in acid-resistant reacting kettle carrying out acid-leaching reaction with the hydrochloric acid that concentration is 5wt%, reaction temperature is 180 DEG C,
Reaction pressure 1.5MPa, response time 1h, acid coal liquid-solid ratio be 1L/Kg, product after filtration washing, the mellow lime branch of coal
Dividing removing, still contain the ash of 19.02%, wherein dioxide-containing silica is 12.7%, and major impurity element is ferrum and calcium etc..De-
Culm, through 1400 DEG C of high-temperature calcinations, carries out mixing to mix joining with the ratio of mash form with after-smithing petroleum coke 40:70 in mass ratio, logical
Crossing grain size distribution, kneading, molding and calcining process, prepare siliceous prebaked anode sample, its true density is 1.91g/cm3, volume
Density is 1.46g/cm3, resistivity is 82.24 μ Ω m, and comprcssive strength is 30.1MPa, and in anode, the content of silicon dioxide is 4.0%,
When electrolytic experiment, owing to containing higher impurity element in anode, anode consumption substantially and has slag-off phenomenon, electrolytic production
In do not contain only silicon, possibly together with the impurity such as ferrum and titanium.
Claims (9)
1. the method for an electrolytic preparation alusil alloy, it is characterised in that during electrolytic preparation alusil alloy, uses the carbon anode prepared at interior raw material by coal to comprise the technical steps that as the silicon source in alusil alloy, the preparation of described carbon anode:
A., coal powder is broken to below 100 mesh, and adding mass percent concentration is that the hydrochloric acid of 10-37% carries out acid-leaching reaction at 120-220 DEG C, and acid-leaching reaction dissolution pressure is 0.3-3MPa, through solid-liquid separation and washing after reaction completely, obtains clean coal and pickle liquor；
B. the clean coal of step a gained is carried out coal after calcining is forged at 1200-2000 DEG C；
C. with siliceous rear coal and the after-smithing petroleum coke forged as aggregate, with coal pitch of agglomerant kneading, through molding and roasting, carbon anode is prepared.
Method the most according to claim 1, it is characterised in that in described step a, coal feedstock includes anthracite, bituminous coal and/or brown coal.
Method the most according to claim 1, it is characterised in that hydrochloric acid is 0.5-5L/Kg with the addition ratio of coal.
Method the most according to claim 1, it is characterised in that the described acid-leaching reaction time is 0.5-5.0 hour.
Method the most according to claim 1, it is characterised in that siliceous forge rear coal and join raw material as producing mixing of pre-baked carbon anode, it mixes dosage and after-smithing petroleum coke mass ratio is 5:95-50:50.
Method the most according to claim 1, it is characterised in that with coal pitch of agglomerant kneading process in described step c, the quality of binding agent accounts for the 13%-18% of anode paste gross weight.
Method the most according to claim 1, it is characterised in that in described step b., calcination time 1-3 hour.
Method the most according to claim 1, it is characterised in that described pickle liquor is evaporated crystallization, obtains solid-state chloride, collects the hydrogen chloride gas that evaporation process produces simultaneously, after absorbing with water, returns to step a for acid-leaching reaction.
9. according to the method described in any one of claim 1-8, it is characterized in that, adding mass percent concentration in described step a is to carry out acid-leaching reaction at the hydrochloric acid of 15-25%, 180-200 DEG C, acid-leaching reaction dissolution pressure is 1.0-2.0MPa, and the acid-leaching reaction time is 2-3 hour.
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Citations (3)
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| US6478945B1 (en) * | 1998-12-17 | 2002-11-12 | Nippon Light Metal Co., Ltd. | Method for producing highly pure aluminum primary base metal |
| CN101343751A (en) * | 2008-08-15 | 2009-01-14 | 中国矿业大学 | Electrolytic aluminium anode carbon block and manufacture method thereof |
| CN102146570A (en) * | 2011-02-26 | 2011-08-10 | 王建军 | Method for producing aluminum anode by using waste cathode carbon block of aluminum cell |
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2014
- 2014-12-26 CN CN201410830210.3A patent/CN104532300B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6478945B1 (en) * | 1998-12-17 | 2002-11-12 | Nippon Light Metal Co., Ltd. | Method for producing highly pure aluminum primary base metal |
| CN101343751A (en) * | 2008-08-15 | 2009-01-14 | 中国矿业大学 | Electrolytic aluminium anode carbon block and manufacture method thereof |
| CN102146570A (en) * | 2011-02-26 | 2011-08-10 | 王建军 | Method for producing aluminum anode by using waste cathode carbon block of aluminum cell |
Non-Patent Citations (1)
| Title |
|---|
| 无烟煤制作铝电解炭阳极的研究;任耀剑;《中国博士学位论文全文数据库工程科技Ⅰ辑 》;20100215;第B023-15页 * |
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