CN103359737B - A kind of industrial silicon is to the complete liquid continuous production method of medium melting - Google Patents
A kind of industrial silicon is to the complete liquid continuous production method of medium melting Download PDFInfo
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- CN103359737B CN103359737B CN201310315024.1A CN201310315024A CN103359737B CN 103359737 B CN103359737 B CN 103359737B CN 201310315024 A CN201310315024 A CN 201310315024A CN 103359737 B CN103359737 B CN 103359737B
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Abstract
The invention belongs to medium smelting technique field, particularly a kind of industrial silicon is to the complete liquid continuous production method of medium melting.Its method is as follows: (1) carries out the smelting of industrial silicon in mineral hot furnace, is imported in silicon bag by liquid-state industrial silicon, and carries out oxygen blast process to this liquid-state industrial silicon; (2) in the plumbago crucible in medium frequency induction melting furnace, add the 30-50% of slag agent quality, start medium frequency induction melting furnace, to plumbago crucible pre-heating temperature elevation; (3) the liquid-state industrial silicon in silicon bag is poured in plumbago crucible, regulate the temperature of medium frequency induction melting furnace simultaneously; (4) in plumbago crucible, add the agent of residue mixing slag; (5) in medium frequency induction melting furnace, medium fusion process is carried out.Device used, the lower end of the mineral hot furnace in smelting industrial silicon device has out silicon mouth, and the silicon mouth side that goes out of mineral hot furnace is provided with purlin car; Purlin car is connected with silicon bag by hoist cable; The below of purlin car is placed with the medium frequency induction melting furnace in medium melting equipment.
Description
Technical field
The invention belongs to medium smelting technique field, particularly a kind of industrial silicon is to the complete liquid continuous production method of medium melting and device thereof.
Background technology
In energy scarcity, the society advocating low-carbon environment-friendly, sun power, as a kind of environmental protection new forms of energy, has great using value.Solar energy converting can be electric energy by solar cell, and solar grade polycrystalline silicon material is the important source material of solar cell, and therefore, the technology of preparing of solar grade polycrystalline silicon material is even more important.At present, the main technological route preparing solar grade polycrystalline silicon material in world wide has: improved Siemens, silane thermal decomposition process, metallurgy method.Wherein the principle of improved Siemens is exactly reduce high-purity trichlorosilane by High Purity Hydrogen on the HIGH-PURITY SILICON core of about 1100 DEG C, generates polysilicon deposition on silicon core.But improved Siemens energy consumption is high, seriously polluted, belong to American-European old technology of eliminating.Silane thermal decomposition process is exactly silane (SiH
4) thermolysis prepares the method for polysilicon, but dangerous large (silane is inflammable and explosive) during the operation of this explained hereafter, comprehensive production cost are higher.Metallurgy method mainly comprises: electron-beam process, beam-plasma smelting process, directional solidification method, medium method, electrolytic process, carbothermic method etc.The mode purifying polycrystalline silicon of medium refining is utilized to be considered to be in suitability for industrialized production the most feasible, even if a medium is difficult to reach the content requirement of polycrystalline silicon used for solar battery material to B impurity, but analyze from operability and cost performance, selection best beyond doubt.
Traditional metallurgy method technical process take industrial silicon as raw material, utilize medium melting technology removal B impurity wherein, two kinds independently technique cannot realize effective linking, industrial silicon after oxygen blast process needs just can be used to carry out medium melting through processes such as fragmentation, packaging, transports, and in medium fusion process, industrial silicon surface oxidation part also needs through screening, the loss of raw material can be caused like this, need during secondary fusion to consume a large amount of electric energy simultaneously, cost is increased considerably.
Summary of the invention
The object of the invention is to overcome above-mentioned not enough problem, the complete liquid continuous production method of a kind of industrial silicon to medium melting and device are provided, the method and device are by combining industrial silicon production technique with medium smelting technique, realize from silicon ore deposit to Boron contents lower than the process of the complete liquid continuous prodution of 0.3ppm, the cost of industrial silicon fragmentation, packaging, transport and secondary fusion process can be saved, technique is more succinct, and polysilicon quality can better be ensured.
A kind of industrial silicon of the present invention is to the complete liquid continuous production method of medium melting, and its method is as follows:
(1) in mineral hot furnace, carry out the smelting of industrial silicon, finally obtain liquid-state industrial silicon, liquid-state industrial silicon is imported in silicon bag, and oxygen blast process is carried out to this liquid-state industrial silicon;
(2) in the plumbago crucible in medium frequency induction melting furnace, add the 30-50% of slag agent quality, start medium frequency induction melting furnace, to plumbago crucible pre-heating temperature elevation;
(3) the liquid-state industrial silicon in silicon bag is poured in plumbago crucible, regulate the temperature of medium frequency induction melting furnace simultaneously, ensure that liquid-state industrial silicon does not solidify;
(4) in plumbago crucible, add the agent of residue mixing slag;
(5) in medium frequency induction melting furnace, medium fusion process is carried out.
In the oxygen blast process of step (1), the amount of being blown into of oxygen is preferably 40-60kg/h.
Slag agent in step (2) is the mixture of the calcium oxide of arbitrary proportion, Calcium Fluoride (Fluorspan), titanium dioxide, silicon-dioxide and water glass.This several material is all the conventional slag former in polycrystalline silicon medium fusion process, and preferred version of the present invention is the arbitrary combination of this several material.
The temperature of the intensification in step (2) is preferably 800-1000 DEG C.
Temperature in step (3) regulates preferably to 1414-1450 DEG C.
Industrial silicon is to the complete liquid continuous production method of a medium melting device used, and the lower end of the mineral hot furnace in smelting industrial silicon device has out silicon mouth, and the silicon mouth side that goes out of mineral hot furnace is provided with purlin car; Purlin car is connected with silicon bag by hoist cable; The below of purlin car is placed with the medium frequency induction melting furnace in medium melting equipment.
Preferably dust removal installation is installed above induction melting furnace.
In process of the present invention, calcium and aluminium impurity are removed in the effect that liquid towards industrial silicon carries out oxygen blast process, ensure that liquid-state industrial silicon does not solidify, when the liquid-state industrial silicon in silicon bag is removed, temperature reaches more than 1500 DEG C simultaneously, step carries out preheating to plumbago crucible in (2), temperature is preferably 800-1000 DEG C, now regulates the temperature of medium frequency induction melting furnace, makes it reach on 1414 DEG C gradually, ensure that, when energy consumption is minimum, liquid-state industrial silicon does not solidify.Meanwhile, first spread the agent of one deck slag, then add the way of liquid-state industrial silicon in operation, the liquid-state industrial silicon being conducive to minimizing high calorie, to the damage of plumbago crucible, reduces the infringement to equipment, extends the work-ing life of plumbago crucible.
Advantage of the present invention is: can eliminate the fragmentation of industrial silicon, packaging and transportation completely, eliminate again the melting process of silicon material simultaneously, power consumption can save 5000 KWhs/ton, production cost reduces 3000-5000 yuan/ton, and makes be increased to 10-12 time/by 8 times/the work-ing life of plumbago crucible.
Accompanying drawing explanation
Fig. 1 is a kind of industrial silicon to the complete liquid continuous production method of medium melting device schematic diagram used.
In figure, 1, mineral hot furnace, 2, purlin car, 3, dust removal installation, 4, silicon bag, 5, medium frequency induction melting furnace
Embodiment
Describe the present invention in detail below in conjunction with specific embodiment, but the present invention is not limited to specific embodiment.
Embodiment 1:
(1) in mineral hot furnace 1, first carry out the smelting of industrial silicon, finally obtain liquid-state industrial silicon, control purlin car 2, imported in silicon bag 4 by the 100kg liquid-state industrial silicon taken out, and carry out oxygen blast process to this liquid-state industrial silicon, the oxygen amount of being blown into is 40kg/h.
(2) slag agent total mass is 100kg, comprises 10kg titanium dioxide, the water glass of 30kg silicon-dioxide and 60kg; Start dust removal installation 3, in the plumbago crucible in medium frequency induction melting furnace 5, add the agent of 30kg slag, start medium frequency induction melting furnace 5, to plumbago crucible pre-heating temperature elevation to 800 DEG C.
(3) control purlin car 2, the liquid-state industrial silicon in silicon bag 4 is poured in plumbago crucible, regulate the temperature of medium frequency induction melting furnace 5 to reach 1430 DEG C simultaneously, ensure that liquid-state industrial silicon does not solidify.
(4) in plumbago crucible, remaining 60kg slag agent is added.
(5) in medium frequency induction melting furnace 5, medium fusion process is carried out.
Embodiment 2:
(1) in mineral hot furnace 1, first carry out the smelting of industrial silicon, finally obtain liquid-state industrial silicon, control purlin car 2, imported in silicon bag 4 by the 150kg liquid-state industrial silicon taken out, and carry out oxygen blast process to this liquid-state industrial silicon, the oxygen amount of being blown into is 60kg/h.
(2) slag agent total mass is 150kg, comprises 15kg titanium dioxide, 15kg silicon-dioxide, the water glass of 10kg Calcium Fluoride (Fluorspan) and 60kg; Start dust removal installation 3, in the plumbago crucible in medium frequency induction melting furnace 5, add the agent of 70kg slag, start medium frequency induction melting furnace 5, to plumbago crucible pre-heating temperature elevation to 900 DEG C.
(3) control purlin car 2, the liquid-state industrial silicon in silicon bag 4 is poured in plumbago crucible, regulate the temperature of medium frequency induction melting furnace 5 to reach 1450 DEG C simultaneously, ensure that liquid-state industrial silicon does not solidify.
(4) in plumbago crucible, remaining 80kg slag agent is added.
(5) in medium frequency induction melting furnace 5, medium fusion process is carried out.
In sum, the present invention can eliminate the fragmentation of industrial silicon, packaging and transportation completely, eliminate again the melting process of silicon material simultaneously, power consumption can save 5000 KWhs/ton, production cost reduces 3000-5000 yuan/ton, and makes be increased to 10-12 time/by 8 times/the work-ing life of plumbago crucible.
Claims (4)
1. industrial silicon is to a complete liquid continuous production method for medium melting, it is characterized in that method is as follows:
(1) in mineral hot furnace (1), carry out the smelting of industrial silicon, finally obtain liquid-state industrial silicon, liquid-state industrial silicon is imported in silicon bag (4), and oxygen blast process is carried out to this liquid-state industrial silicon;
(2) in the plumbago crucible in medium frequency induction melting furnace (5), add the 30-50% of slag agent quality, start medium frequency induction melting furnace (5), to plumbago crucible pre-heating temperature elevation to 800 ~ 1000 DEG C;
(3) the liquid-state industrial silicon in silicon bag (4) is poured in plumbago crucible, regulate the temperature of medium frequency induction melting furnace (5) simultaneously, ensure that liquid-state industrial silicon does not solidify;
(4) in plumbago crucible, add the agent of residue mixing slag;
(5) in medium frequency induction melting furnace (5), medium fusion process is carried out.
2. a kind of industrial silicon according to claim 1 is to the complete liquid continuous production method of medium melting, it is characterized in that, in the oxygen blast process of described step (1), the amount of being blown into of oxygen is 40-60kg/h.
3. a kind of industrial silicon according to claim 1 is to the complete liquid continuous production method of medium melting, it is characterized in that, the slag agent in described step (2) is the mixture of the calcium oxide of arbitrary proportion, Calcium Fluoride (Fluorspan), titanium dioxide, silicon-dioxide and water glass.
4. a kind of industrial silicon according to claim 1 is to the complete liquid continuous production method of medium melting, it is characterized in that: the temperature in described step (3) is adjusted to 1414-1450 DEG C.
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| CN201310315024.1A CN103359737B (en) | 2013-07-23 | 2013-07-23 | A kind of industrial silicon is to the complete liquid continuous production method of medium melting |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102139877A (en) * | 2011-01-26 | 2011-08-03 | 山东盛华光伏材料有限公司 | Method for removing boron and phosphorus impurities in industrial silicon by ferrous compounds |
| CN102241400A (en) * | 2011-05-17 | 2011-11-16 | 云南永昌硅业股份有限公司 | External refining method of industrial silicon |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102139877A (en) * | 2011-01-26 | 2011-08-03 | 山东盛华光伏材料有限公司 | Method for removing boron and phosphorus impurities in industrial silicon by ferrous compounds |
| CN102241400A (en) * | 2011-05-17 | 2011-11-16 | 云南永昌硅业股份有限公司 | External refining method of industrial silicon |
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