CN102241400A - External refining method of industrial silicon - Google Patents
External refining method of industrial silicon Download PDFInfo
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- CN102241400A CN102241400A CN2011101277179A CN201110127717A CN102241400A CN 102241400 A CN102241400 A CN 102241400A CN 2011101277179 A CN2011101277179 A CN 2011101277179A CN 201110127717 A CN201110127717 A CN 201110127717A CN 102241400 A CN102241400 A CN 102241400A
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Abstract
The invention discloses an external refining method of industrial silicon. According to the method, compressed air and oxygen are introduced, so that oxidation of aluminum in silicon liquid is accelerated to form oxidized slag in the presence of refining impurity remover calspar; impurity remover calspar has decomposition reaction in the high-temperature silicon liquid to generate calcium oxide; calcium oxide reacts with aluminum in silicon water so as to oxidize and remove aluminum (Al); and the generated aluminum-containing slag easily floats up to achieve the aim of separating and removing slag from liquid. By the adoption of the method disclosed by the invention, the aluminum content can be reduced, the quality of an industrial silicon product can be enhanced and the markedemands on low-aluminum industrial silicon products and different models of special industrial silicon differential products can be met.
Description
Technical field
The present invention relates to a kind of industrial silicon secondary refining method.
Background technology
The industrial silicon external refining is to adopt oxidation refining method, be that aerating oxygen and air gas mixture are carried out refining, refining process in fact also is a slagging process, it is the balance refining process of a slag system, this method is to realize removing impurity by the oxidized reaction process of impurity, belong to a kind of selective oxidation, depend merely on only silicon in the product, aluminium, the calcium ternary alloy carries out refining, because the avidity maximum of calcium and oxygen more easily is removed, do not reach balance purified purpose, the silicon liquid temp is higher in addition, on average up to 1650 ℃, under hot conditions, the avidity of aluminium and oxygen is relatively poor, the oxidation removal that is unfavorable for aluminium, so the decreasing ratio of aluminium can only reach 40% in the product; Along with the progress that science and technology is produced, client is to the industrial silicon foreign matter content, and is especially more and more stricter to the requirement of aluminium, so the refining of aluminium is deviate from weak effect and will be had a strong impact on the industrial silicon quality product.
Summary of the invention
The objective of the invention is to overcome the deficiency that above-mentioned prior art exists, provide a kind of industrial silicon furnace outer purified method, can reduce aluminium content in the outer refining process of this industrial silicon furnace, improve the industrial silicon quality product, solve the problem of the industrial silicon differentiation product of the low aluminium industrial silicon product of market demand and the special different trades mark.
The present invention feeds pressurized air and oxygen, assorted agent calcium stone is taken off in additional refining, make the aluminium in the silicon liquid must be in promote the oxidation, form oxidation sludge, utilization is taken off assorted agent calcium stone decomposition reaction generation calcium oxide is taken place in high temperature silicon liquid, aluminium in calcium oxide and the silicon water reacts, and removes thereby help the Al oxidation, and reaction formula is:
CaCO
3＝CaO+CO
2
2Al+3CaO＝Al
2O
3+3Ca
The aluminium slag that contains that generates in the formula is easy to come-up in silicon liquid, reach slag liquid and separate the purpose of deviating from.Take off assorted agent calcium stone add-on and calculate adding in proportion, to meet the requirement of slag system balance according to calcium, aluminium content in the silicon liquid.
The method of refining that takes off assorted agent calcium stone by interpolation has improved slag fall, makes the decreasing ratio of aluminium in the silicon liquid obtain by a relatively large margin raising.
The inventive method is applicable to employing oxygen and the outer refining process of air purified industrial silicon furnace, and the present invention is simple to operate, and cost is lower.
Embodiment
The hot stove in ore deposit is emitted silicon content and is entered in the oxygen blown silicon bag in bottom greater than 98% molten silicon liquid, before not flowing into the silicon bag, opens in silicon water the pressurized air of 350L/min, and guarantee that tracheae is unimpeded, after silicon liquid flows into the silicon bag, aerating oxygen, the control oxygen flow is 700L/min, when the silicon liquid measure reaches 2000Kg, adopt the digital display temperature measurer to measure the silicon liquid temp, control silicon liquid temp adds calcium stone 33-50Kg by silicon liquid per ton under 1460-1520 ℃ condition, must guarantee during operation that the calcium stone that adds all is in molten state, otherwise it is invalid to add calcium stone, when treating that the silicon liquid measure reaches 5000kg in the silicon bag, once more silicon liquid is carried out thermometric, adopt the cold silicon reduction silicon liquid temp of increase or adjusting bubbling air+oxidation ratio to strengthen oxidizing reaction and improve the silicon liquid temp, the silicon liquid temp is controlled at about 1460-1520 ℃, the temperature adjustment is suitable, after refining 0.5-1 hour, reduce aerating oxygen+air tolerance, air capacity is 100L/min, oxygen is 300L/min, continue again to treat in refining 5-10 minute that refining finishes when the layering of slag liquid appears in silicon liquid, with the driving silicon bag of slinging, silicon liquid evenly slowly poured into carry out cooled and solidified in the silicon ingot mould, the oxidation sludge that refining produces is poured a shelves slag device of wrapping by silicon in the ingot mould process at silicon liquid and is stayed in the silicon bag artificial the removing and handle.
The contrast of traditional refining and two kinds of method impurity removals of refining of the present invention situation will be described by five practical situation of following table below:
Claims (1)
1. the outer purified method of an industrial silicon furnace, it is characterized in that: the hot stove in ore deposit is emitted silicon content and is entered in the oxygen blown silicon bag in bottom greater than 98% molten silicon liquid, before not flowing into the silicon bag, silicon water feeds the pressurized air of 350L/min, after silicon liquid flows into the silicon bag, feed the oxygen of 700L/min, when the silicon liquid measure reaches a certain amount of, control silicon liquid temp takes off assorted agent calcium stone 33-50Kg by silicon liquid adding per ton under 1460-1520 ℃ condition, after refining 0.5-1 hour, being decreased to and feeding air supply is 100L/min, oxygen is 300 L/min, refining finishes when treating that the layering of slag liquid appears in silicon liquid in refining 5-10 minute again, with the driving silicon bag of slinging, silicon liquid evenly slowly poured into carry out cooled and solidified in the silicon ingot mould.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101277179A CN102241400A (en) | 2011-05-17 | 2011-05-17 | External refining method of industrial silicon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101277179A CN102241400A (en) | 2011-05-17 | 2011-05-17 | External refining method of industrial silicon |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102241400A true CN102241400A (en) | 2011-11-16 |
Family
ID=44959685
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101277179A Pending CN102241400A (en) | 2011-05-17 | 2011-05-17 | External refining method of industrial silicon |
Country Status (1)
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| CN (1) | CN102241400A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583389A (en) * | 2012-03-05 | 2012-07-18 | 昆明理工大学 | Method for purifying industrial silicon through external refining |
| CN102826551A (en) * | 2012-09-17 | 2012-12-19 | 云南永昌硅业股份有限公司 | Blow-in method for long-term shutdown maintenance of metallic silicon ore heating furnace |
| CN103359737A (en) * | 2013-07-23 | 2013-10-23 | 青岛隆盛晶硅科技有限公司 | All-liquid continuous production method from industrial silicon to medium melting and apparatus thereof |
| CN107311182A (en) * | 2017-06-30 | 2017-11-03 | 昆明理工大学 | A kind of device and method thereof of industrial silicon melt external refining purification |
| CN107352546A (en) * | 2017-06-30 | 2017-11-17 | 昆明理工大学 | A kind of devices and methods therefor of silicon melt external refining |
| CN114671438A (en) * | 2022-03-31 | 2022-06-28 | 新疆西部合盛硅业有限公司 | Method for automatically controlling oxygen blowing refining by interlocking weight and temperature |
-
2011
- 2011-05-17 CN CN2011101277179A patent/CN102241400A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583389A (en) * | 2012-03-05 | 2012-07-18 | 昆明理工大学 | Method for purifying industrial silicon through external refining |
| CN102826551A (en) * | 2012-09-17 | 2012-12-19 | 云南永昌硅业股份有限公司 | Blow-in method for long-term shutdown maintenance of metallic silicon ore heating furnace |
| CN103359737A (en) * | 2013-07-23 | 2013-10-23 | 青岛隆盛晶硅科技有限公司 | All-liquid continuous production method from industrial silicon to medium melting and apparatus thereof |
| CN103359737B (en) * | 2013-07-23 | 2016-01-13 | 青岛隆盛晶硅科技有限公司 | A kind of industrial silicon is to the complete liquid continuous production method of medium melting |
| CN107311182A (en) * | 2017-06-30 | 2017-11-03 | 昆明理工大学 | A kind of device and method thereof of industrial silicon melt external refining purification |
| CN107352546A (en) * | 2017-06-30 | 2017-11-17 | 昆明理工大学 | A kind of devices and methods therefor of silicon melt external refining |
| CN114671438A (en) * | 2022-03-31 | 2022-06-28 | 新疆西部合盛硅业有限公司 | Method for automatically controlling oxygen blowing refining by interlocking weight and temperature |
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Application publication date: 20111116 |