CN104532300A - Electrolytic preparation method of aluminum-silicon alloy - Google Patents
Electrolytic preparation method of aluminum-silicon alloy Download PDFInfo
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- CN104532300A CN104532300A CN201410830210.3A CN201410830210A CN104532300A CN 104532300 A CN104532300 A CN 104532300A CN 201410830210 A CN201410830210 A CN 201410830210A CN 104532300 A CN104532300 A CN 104532300A
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- carbon anode
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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
The invention relates to an electrolytic preparation method of an aluminum-silicon alloy, which adopts a carbon anode prepared from coal as a silicon source in the aluminum-silicon alloy. The carbon anode is prepared by the following steps: reacting coal with a hydrochloric acid solution, carrying out solid-liquid separation to obtain silicious clean coal, calcining to obtain calcined coal, doping with calcined petroleum coke, adding coal pitch, kneading, forming and roasting to prepare the carbon anode with a certain silicon content, which can be used for electrolytic preparation of the aluminum-silicon alloy. The acid leaching filtrate is evaporated to obtain solid chloride and hydrogen chloride gas, and the hydrogen chloride gas is collected for cyclic leaching of hydrochloric acid. The method has the characteristics of sufficient raw material sources, high comprehensive utilization value of coal, short technical process, low production cost, low residue amount, recyclable hydrochloric acid and the like, provides a technical route for preparing the novel carbon anode from coal, and has wide application prospects.
Description
Technical field
The present invention relates to a kind of method of electrolytic preparation aluminum silicon alloy.
Background technology
Aluminum silicon alloy widespread use and communications and transportation, electric power, automobile and aeronautical light field, generally adopt fine aluminium and pure silicon mix-melting method to produce aluminum silicon alloy at present, alloy production link is many, and the cycle is long, and energy consumption is high, and scale of investment is large.
China is the country that petroleum resources are in short supply, and the petroleum import dependency degree of China reaches about 50%-60% in recent years, and along with the anxiety of petroleum resources, the refinery coke of one of carbon anode starting material relying on oil production also becomes in short supply.
China has quite abundant coal reserves, also cheap more than refinery coke in price, uses coal to prepare aluminum carbon anode in raw materials cost, has obviously advantage.But, because aluminum carbon anode has strict requirement to ash content, and usually containing higher ash content in coal, therefore, need to carry out deliming process to coal.At present, although utilize the technology such as acid-base method, hydrogen fluoride, solvent extraction and oil briquetting floating method the ash content in coal can be reduced to less than 1%, 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 ", the oxide compounds such as aluminum oxide, silicon oxide and titanium oxide are added to electrolyzer Direct Electrolysis and produce aluminium, silicon and titanium multielement alloy, but the segregation in aluminium liquid of silicon and titanium is serious, current efficiency is low, also causes very large difficulty to the normal production of electrolyzer.
Patent CN101255572A discloses " a kind of method utilizing calcined anthracite to prepare aluminum carbon anode ", and the low grey hard coal selecting ash content to be less than 5% is calcined, and then mixes to join after-smithing petroleum coke and prepare aluminum carbon anode.Because this hard coal does not carry out deliming process, ash content is still higher, so the ratio of petroleum replacing Jiao is lower, in addition, the anthracitic reserves of low ash do not enrich, and the source of raw material is still limited.
Method that patent CN101225530A discloses " low-ash carbonaceous raw material is preparing the application in prebaked anode ", carbon residue after selecting low grey hard coal, bituminous coal, bamboo charcoal, charcoal, plastic waste or waste rubber to carbonize is as the auxiliary material producing prebaked anode, the above-mentioned carbon residue ash oontent of patent requirements is no more than 2.8%, under this ash oontent requires, obviously can improve the mixture proportion of carbonaceous raw material, but corresponding low-ash carbonaceous raw material source is more rare.
Patent CN101698947A discloses " a kind of preparation method of aluminium electrolysis carbon anode ", is mixed by flotation de-ash coal calcine with powdery raw petroleum coke, obtained compound calcined coke, is used for replacing part or all of refinery coke and makes aluminum carbon anode.The ash oontent of patent requirements flotation de-ash coal is less than 2.5%, requires very high, only have little a part of coal to satisfy the demands to the washability of coal.
Therefore, current carbon anode used for aluminium electrolysis generally adopts the less carbon material of ash content to produce, and take refinery coke as aggregate, adopts coal-tar pitch as binding agent, is prepared from.And to relate to carbon anode in existing technique be all how to remove all impurity, and what technique is adopted to reduce ash treatment in raw material as much as possible.But for various reasons, the de-ash process deliming efficiency of employing is poor, and the workload of deliming is large.But at present along with the external crude oil with poor quality of China's import and heavy crude proportion constantly rise, cause the supply of high-quality petroleum coke to have decline to a certain degree, thus aggravation aluminium high-quality petroleum coke is in short supply.
Summary of the invention
The object of the present invention is to provide a kind ofly can not need the method for electrolytic preparation aluminum silicon alloy of the carbon anode that the basis of complicated dedusting process obtains.
Technical scheme of the present invention is:
In electrolytic preparation aluminum silicon alloy process, employing be the carbon anode that prepared at interior raw material by coal as the silicon source in aluminum silicon alloy, the preparation of described carbon anode comprises following processing step:
A. coal powder is broken to below 100 orders, 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 stripping pressure is 0.3-3Mpa, through solid-liquid separation and washing after reacting completely, obtains clean coal and pickling liquor;
B. by the clean coal of step a gained 1200-2000 DEG C carry out calcining obtain forging after coal;
C. with siliceous rear coal and the after-smithing petroleum coke forged for aggregate, with coal pitch of agglomerant kneading, through shaping and roasting, obtained carbon anode.
In described step a, coal feedstock comprises and has hard coal, bituminous coal and/or brown coal.
The add-on ratio of hydrochloric acid and coal is 0.5-5L/Kg.
The described acid-leaching reaction time is 0.5-5.0 hour.
Siliceous forge rear coal as production mixing of pre-baked carbon anode join raw material, it mixes dosage and 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. walks pickling liquor and carries out evaporative crystallization, obtains solid-state chloride, collects the hydrogen chloride gas that evaporative process produces simultaneously, after absorbing, returns to step a for acid-leaching reaction with water.
Particularly preferably be in the present invention in described step a and add the hydrochloric acid that mass percent concentration is 15-25%, carry out acid-leaching reaction at 180-200 DEG C, acid-leaching reaction stripping pressure is 1.0-2.0Mpa, and the acid-leaching reaction time is 2-3 hour.
Coal feedstock hard coal, bituminous coal and/or brown coal etc. in step a of the present invention; In coal feedstock, dioxide-containing silica is 3% ~ 50% to be advisable.By making silicon optionally be retained in coal after acid leaching process process of the present invention, and other impurity is removed.
The present invention selects coal as raw material, the coal of almost all kinds all can be selected, adopt the ash impurities in the method removal coal of direct acidleach, adopt reactor 120-220 DEG C of leaching during acidleach, one step deliming removal of impurity can reach more than 95%, simplify de-ash process flow process, reduce production cost; Simultaneously, the present invention is also by adding the art breading of hydrochloric acid, and the control of relevant parameters, can ensure that in coal, other impurity element removes completely simultaneously, silicon composition is made to be retained in de-ash coal, for this siliceous clean coal characteristic, after calcining, Substitute For Partial refinery 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, ash oontent is high, but also the valuable constituent silicon in ash content of coal is fully utilized, in de-ash coal, siliceous composition is no longer considered to impurity, can increase the ratio of replacing refinery coke.In addition, the link that follow-up fine aluminium and pure silicon melt the standby aluminum silicon alloy of preparation is decreased.The present invention is while realizing coal replacement part refinery coke, utilize silicon composition intrinsic in coal, if be selectively retained in coal by this part element silicon, while alleviating the burden of deliming operation, be lowered into product cost, and produce aluminum silicon alloy by the carbon anode Direct Electrolysis that method of the present invention prepares, produce for aluminum silicon alloy, effectively prevent and generally adopt fine aluminium and pure silicon mix-melting method to produce aluminum silicon alloy at present, alloy production link is many, 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, has widened the scope of application of coal resources, the production cost of carbon anode can be made significantly to decline, and expands the raw material availability of carbon industry; On the other hand, the making of carbon anode and the production cost of aluminum silicon alloy can be reduced simultaneously; The carbon anode obtained by form of the present invention uses this de-ash coal Substitute For Partial refinery coke to prepare carbon anode, the prepared siliceous carbon anode of coal of mixing can be used for Direct Electrolysis and goes out aluminum silicon alloy, compared with original technique, eliminate middle-chain, energy-saving and cost-reducing object can be reached.Prepare Novel carbon anode for coal and provide processing technology routine, have broad application prospects; There is good economic benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is for the process flow sheet of Electrolytic Al-Si Alloys carbon anode prepared by raw material with sour de-ash coal;
Embodiment
Be described further below in conjunction with the drawings and specific embodiments, but the present invention is not therefore subject to any restriction.
Embodiment 1
Recording hard coal ash content is 32.04%, wherein dioxide-containing silica is 20%, volatilization is divided into 4.97%, pulverized anthracite is broken to below 100 orders, then put into the hydrochloric acid that acid-resistant reacting kettle and concentration are 20wt% and carry out acid-leaching reaction, temperature of reaction is 180 DEG C, reaction pressure 1.5MPa, reaction times 2h, reaction product obtains the clean coal that dioxide-containing silica is 21.5% after washing after filtration, after measured, in hard coal, the decreasing ratio of other metallic impurity reaches more than 95% in addition to silicon, de-ash coal is through 1400 DEG C of high-temperature calcinations, with mash form and after-smithing petroleum coke in mass ratio the ratio of 40:60 carry out mixing to mix joining, pass through grain size distribution, kneading, shaping and calcining process, obtained siliceous prebaked anode sample, its true density is 1.95g/cm
3, volume density is 1.49g/cm
3, resistivity is 62.36 μ Ω m, ultimate compression strength 34.5MPa, and wherein dioxide-containing silica is 8.6%, for electrolytic preparation aluminum silicon alloy, electrolytic production silicon from aluminum-silicon alloy content is 2.0%.
Embodiment 2
Recording hard coal ash content is 17.14%, wherein dioxide-containing silica is 7.8%, volatilization is divided into 4.42%, bituminous coal powder is broken to below 100 orders, then put into the hydrochloric acid that acid-resistant reacting kettle and concentration are 25wt% and carry out acid-leaching reaction, temperature of reaction is 200 DEG C, reaction pressure 2.0MPa, reaction times 2h, after reaction product is washed after filtration, obtain the clean coal that dioxide-containing silica is 8.6%, de-ash coal is through 1500 DEG C of high-temperature calcinations, with mash form and after-smithing petroleum coke in mass ratio the ratio of 20:80 carry out mixing to mix joining, pass through grain size distribution, kneading, shaping and calcining process, obtained siliceous prebaked anode sample, its true density is 1.94g/cm
3, volume density is 1.49g/cm
3, resistivity is 68.23 μ Ω m, and ultimate compression strength is 35.3MPa, and wherein dioxide-containing silica is 1.73%, for electrolytic preparation aluminum silicon alloy, electrolytic production silicon from aluminum-silicon alloy content is 0.40%.
Embodiment 3
Recording bituminous coal ash content is 18.75%, wherein dioxide-containing silica is 5.9%, volatilization is divided into 22.28%, coal dust is broken to below 100 orders, then put into the hydrochloric acid that acid-resistant reacting kettle and concentration are 37wt% and carry out acid-leaching reaction, temperature of reaction is 180 DEG C, reaction pressure 1.5MPa, reaction times 2.5h, after reaction product is washed after filtration, obtain the clean coal that dioxide-containing silica is 6.7%, de-ash coal is through 1500 DEG C of high-temperature calcinations, with mash form and after-smithing petroleum coke in mass ratio the ratio of 30:70 carry out mixing to mix joining, pass through grain size distribution, kneading, shaping and calcining process, obtained siliceous prebaked anode sample, its true density is 1.91g/cm
3, volume density is 1.46g/cm
3, resistivity is 75.86 μ Ω m, and ultimate compression strength is 30.7MPa, and wherein dioxide-containing silica is 2.0%, for electrolytic preparation aluminum silicon alloy, after electrolysis, product silicon from aluminum-silicon alloy content is 0.47%.
Embodiment 4
Recording bituminous coal ash content is 28.60%, wherein dioxide-containing silica is 11.42%, volatilization is divided into 17.75%, coal dust is broken to below 200 orders, then put into the hydrochloric acid that acid-resistant reacting kettle and concentration are 37wt% and carry out acid-leaching reaction, temperature of reaction is 180 DEG C, reaction pressure 1.5MPa, reaction times 3h, after reaction product is washed after filtration, obtain the clean coal that dioxide-containing silica is 13.50%, de-ash coal is through 1400 DEG C of high-temperature calcinations, with mash form and after-smithing petroleum coke in mass ratio the ratio of 30:70 carry out mixing to mix joining, pass through grain size distribution, kneading, shaping and calcining process, obtained siliceous prebaked anode sample, its true density is 1.89g/cm
3, volume density is 1.44g/cm
3, resistivity is 80.13 μ Ω m, and ultimate compression strength is 30.2MPa, and wherein dioxide-containing silica is 4.0%, for electrolytic preparation aluminum silicon alloy, after electrolysis, product silicon from aluminum-silicon alloy content is 0.9%
Embodiment 5
Record lignite ash and be divided into 12.64%, wherein dioxide-containing silica is 3.12%, volatilization is divided into 43.75%, coal dust is broken to below 200 orders, then put into the hydrochloric acid that acid-resistant reacting kettle and concentration are 10wt% and carry out acid-leaching reaction, temperature of reaction is 180 DEG C, reaction pressure 1.5MPa, reaction times 3.5h, after reaction product is washed after filtration, obtain the clean coal that dioxide-containing silica is 3.3%, de-ash coal is through 1500 DEG C of high-temperature calcinations, with mash form and after-smithing petroleum coke in mass ratio the ratio of 10:90 carry out mixing to mix joining, pass through grain size distribution, kneading, shaping and calcining process, obtained siliceous prebaked anode sample, its true density is 1.97g/cm
3, volume density is 1.50g/cm
3, resistivity is 69 μ Ω m, and ultimate compression strength is 31.6MPa, and wherein dioxide-containing silica is 0.35%, for electrolytic preparation aluminum silicon alloy, after electrolysis, product silicon from aluminum-silicon alloy content is 0.1%.
Comparative example 1
Recording hard coal ash content is 17.14%, wherein dioxide-containing silica is 7.8%, and volatilization is divided into 4.42%, and the granularity selection of coal is below 100 orders, be that the hydrochloric acid of 10wt% carries out acid-leaching reaction at ambient pressure with concentration, temperature of reaction is 90 DEG C, and reaction times 4h, after reaction product is washed after filtration, in coal, ash content only has a small amount of removing, still contain the ash content of 16.02%, wherein dioxide-containing silica is 8.6%, and major impurity element is iron, calcium, magnesium and sodium etc.Pickling coal through 1500 DEG C of high-temperature calcinations, with mash form and after-smithing petroleum coke in mass ratio the ratio of 20:80 carry out mixing to mix joining, by grain size distribution, kneading, shaping and calcining process, obtained prebaked anode sample, its true density is 1.95g/cm
3, volume density is 1.49g/cm
3resistivity is 78.23 μ Ω m, ultimate compression strength is 29.2MPa, wherein dioxide-containing silica is 1.73%, during for electrolytic experiment, owing to containing too high impurity element in anode, anode consumption obviously and have slag-off phenomenon (impurity element has katalysis, anode is caused additionally to consume), not only containing silicon in electrolytic production, also containing the impurity such as iron, titanium.In coal, impurity element removes not thorough, and not only affect anode performance, and cause extra consumption in electrolytic process, in addition, in electrolytic process, contaminating impurity negative electrode aluminium product, increases follow-up removal of impurities work.
Comparative example 2
Recording bituminous coal ash content is 28.60%, wherein dioxide-containing silica is 11.42%, volatilization is divided into 17.75%, coal dust is broken to below 200 orders, then put into the hydrochloric acid that acid-resistant reacting kettle and concentration are 5wt% and carry out acid-leaching reaction, temperature of reaction is 180 DEG C, reaction pressure 1.5MPa, reaction times 1h, sour coal liquid-solid ratio is 1L/Kg, after reaction product is washed after filtration, in coal, ash fraction removes, still contain the ash content of 19.02%, wherein dioxide-containing silica is 12.7%, and major impurity element is iron and calcium etc.De-ash coal through 1400 DEG C of high-temperature calcinations, with mash form and after-smithing petroleum coke in mass ratio the ratio of 40:70 carry out mixing to mix joining, by grain size distribution, kneading, shaping and calcining process, obtained siliceous prebaked anode sample, its true density is 1.91g/cm
3, volume density is 1.46g/cm
3, resistivity is 82.24 μ Ω m, and ultimate compression strength is 30.1MPa, in anode, the content of silicon-dioxide is 4.0%, during for electrolytic experiment, owing to containing higher impurity element in anode, anode consumption obviously and have slag-off phenomenon, not only containing silicon in electrolytic production, also containing the impurity such as iron and titanium.
Claims (9)
1. a method for electrolytic preparation aluminum silicon alloy, is characterized in that, in electrolytic preparation aluminum silicon alloy process, adopt the carbon anode prepared at interior raw material by coal as the silicon source in aluminum silicon alloy, the preparation of described carbon anode comprises following processing step:
A. coal powder is broken to below 100 orders, 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 stripping pressure is 0.3-3Mpa, through solid-liquid separation and washing after reacting completely, obtains clean coal and pickling liquor;
B. by the clean coal of step a gained 1200-2000 DEG C carry out calcining obtain forging after coal;
C. with siliceous rear coal and the after-smithing petroleum coke forged for aggregate, with coal pitch of agglomerant kneading, through shaping and roasting, obtained carbon anode.
2. method according to claim 1, is characterized in that, in described step a, coal feedstock comprises and has hard coal, bituminous coal and/or brown coal.
3. method according to claim 1, is characterized in that, the add-on ratio of hydrochloric acid and coal is 0.5-5L/Kg.
4. method according to claim 1, is characterized in that, the described acid-leaching reaction time is 0.5-5.0 hour.
5. method according to claim 1, is characterized in that, siliceous forge rear coal as production mixing of pre-baked carbon anode join raw material, it mixes dosage and after-smithing petroleum coke mass ratio is 5:95-50:50.
6. method according to claim 1, is characterized 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.
7. method according to claim 1, is characterized in that, in described step b., and calcination time 1-3 hour.
8. method according to claim 1, is characterized in that, described steps d. evaporative crystallization is carried out in middle pickling liquor, obtains solid-state chloride, collects the hydrogen chloride gas that evaporative process produces simultaneously, after absorbing, returns to step a for acid-leaching reaction with water.
9. the method according to any one of claim 1-8, it is characterized in that, add the hydrochloric acid that mass percent concentration is 15-25% in described step a, at 180-200 DEG C, carry out acid-leaching reaction, acid-leaching reaction stripping pressure is 1.0-2.0Mpa, and the acid-leaching reaction time is 2-3 hour.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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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- 2014-12-26 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 |
|---|
| 任耀剑: "无烟煤制作铝电解炭阳极的研究", 《中国博士学位论文全文数据库工程科技Ⅰ辑 》 * |
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