CN108163860A - A kind of industrial silicon rectification systems and refinery practice - Google Patents
A kind of industrial silicon rectification systems and refinery practice Download PDFInfo
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- CN108163860A CN108163860A CN201810174680.7A CN201810174680A CN108163860A CN 108163860 A CN108163860 A CN 108163860A CN 201810174680 A CN201810174680 A CN 201810174680A CN 108163860 A CN108163860 A CN 108163860A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/037—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The present invention provides a kind of industrial silicon rectification systems and refinery practices, belong to industrial silicon production technical field.A kind of industrial silicon rectification systems, including：Mineral hot furnace two-mans ladle, refines furnace module and Temperature-controlled appliance, and the discharge port of mineral hot furnace is connect with the feed inlet two-mand ladle, and two-mans ladle and is configured for carrying out silicon liquid logical oxygen reaction.It refines furnace module and includes refining furnace and petticoat pipe, refining furnace is configured for receiving the silicon liquid after interior logical oxygen reaction of two-maing ladle, and petticoat pipe is used to collect the flue dust of refining furnace, and Temperature-controlled appliance is configured for the temperature in control refining furnace.The system can preferably remove the impurity in industrial silicon, improve the quality of industrial silicon, increase the yield of industrial silicon.
Description
Technical field
The present invention relates to industrial silicon production technical field, in particular to a kind of industrial silicon rectification systems and refining work
Skill.
Background technology
Industrial silicon is also known as metallic silicon, and metallic silicon is the product smelted in mineral hot furnace by silica and carbonaceous reducing agent.Work
Industry silicon is a critically important intermediate products in silicon industrial chain, is the master for manufacturing silicon polished, solar cell and high silicon product
Want raw material.
During smelting industrial silicon, impurity is contained in raw material, these impurity again silica reduction during with
Element silicon is reduced and enters industrial silicon together.In order to improve the quality of industrial silicon, the impurity content in industrial silicon is reduced, usually
By industrial silicon in interior progress oxygen blast slag making of two-maing ladle to remove impurity, so as to obtain the relatively low industrial silicon liquid of impurity content, then into
Row moulding by casting.But silicon liquid temperature in two-maing ladle can decline, and thermodynamic condition be caused to be deteriorated, many impurity can not remove.
Invention content
The purpose of the present invention is to provide a kind of industrial silicon rectification systems, which can preferably remove miscellaneous in industrial silicon
Matter improves the quality of industrial silicon.
The present invention another object be to provide a kind of industrial silicon refinery practice, which can improve the product of industrial silicon
Matter.
The invention is realized in this way：
A kind of industrial silicon rectification systems, including：Mineral hot furnace, two-man ladle, refining furnace and Temperature-controlled appliance, mineral hot furnace go out
Material mouth is connect with the feed inlet two-mand ladle, and is two-mand ladle and is configured for carrying out silicon liquid logical oxygen reaction；
Refining furnace is configured for receiving the silicon liquid after interior logical oxygen reaction of two-maing ladle, and Temperature-controlled appliance is configured for
Control the temperature in refining furnace.
Further, in an embodiment of the present invention：
Refining furnace is provided with multiple, and multiple refining furnaces are correspondingly arranged Temperature-controlled appliance.
Further, in an embodiment of the present invention：
Industrial silicon rectification systems further include petticoat pipe and deduster, and petticoat pipe is used to collect the flue dust of refining furnace, petticoat pipe and dedusting
Device connects.
A kind of industrial silicon refinery practice is mainly carried out using above-mentioned industrial silicon rectification systems, including：By industrial silicon original
Material is smelted to obtain silicon liquid in mineral hot furnace, the silicon liquid in mineral hot furnace is discharged into two-man ladle it is interior carry out logical oxygen reaction, it is anti-through logical oxygen
Silicon liquid after answering is discharged into refining furnace, and the volume of the silicon liquid in refining furnace is refine furnace volume 1/2~2/3, utilizes temperature
Control device controls the temperature in refining furnace at 1500~1750 DEG C, then adds in scrap silicon and calcium class slag former is kneaded
And keep the temperature, the shoddye removed in refining furnace obtains purer silicon liquid.
Further, in an embodiment of the present invention：
Scrap silicon includes polycrystalline monocrystal silicon waste materials particle, polycrystalline monocrystalline silicon Buddha's warrior attendant wire cutting briquetting material, metallic silicon powder
It gives up at least one of fragment with metallic silicon leftover pieces, photovoltaic battery panel.
Further, in an embodiment of the present invention：
Metallic silicon powder includes the dust-removing powder in metallic silicon powder or crushing process.
Further, in an embodiment of the present invention：
Calcium class slag former includes at least one of calcium oxide, calcium hydroxide and calcirm-fluoride.
Further, in an embodiment of the present invention：
Refining temperature is 1600~1750 DEG C.
Further, in an embodiment of the present invention：
The soaking time of silicon liquid is 20~60min.
Further, in an embodiment of the present invention：
The volume of scrap silicon and calcium class slag former is refine furnace volume 1/3~1/2.
The beneficial effects of the invention are as follows：The industrial silicon rectification systems and refinery practice that the present invention is obtained by above-mentioned design,
It is combined by cleaning and cleaning in refining furnace in interior logical oxygen of two-maing ladle, the impurity-eliminating effect of industrial silicon is preferable, and obtained metallic silicon is pure
Degree is higher.Temperature-controlled appliance controls the temperature in refining furnace, comparatively ideal temperature can be provided for refinery practice, favorably
In rejecting impurity.
Description of the drawings
It, below will be to use required in embodiment in order to illustrate more clearly of the technical solution of embodiment of the present invention
Attached drawing be briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not to be seen as
It is the restriction to range, it for those of ordinary skill in the art, without creative efforts, can be with root
Other relevant attached drawings are obtained according to these attached drawings.
Fig. 1 is the schematic diagram for the industrial silicon rectification systems that embodiment of the present invention provides；
Fig. 2 is the flow chart for the industrial silicon refinery practice that embodiment of the present invention provides；
Fig. 3 is the schematic diagram for the industrial silicon rectification systems that embodiment of the present invention provides；
The schematic diagram of another industrial silicon rectification systems that Fig. 4 embodiment of the present invention provides.
Icon：100- industrial silicon rectification systems；110- mineral hot furnaces；120- two-mans ladle；130- refining furnaces；131- petticoat pipes；132-
Deduster；140- Temperature-controlled appliances；141- frequency-conversion control cabinets；142- furnace transformers.
Specific embodiment
Purpose, technical scheme and advantage to make embodiment of the present invention are clearer, implement below in conjunction with the present invention
The technical solution in embodiment of the present invention is clearly and completely described in attached drawing in mode, it is clear that described reality
The mode of applying is the embodiment of a part of embodiment of the present invention rather than whole.Based on the embodiment in the present invention, ability
The every other embodiment that domain those of ordinary skill is obtained without creative efforts, belongs to the present invention
The range of protection.
Therefore, the detailed description of the embodiments of the present invention to providing in the accompanying drawings is not intended to limit requirement guarantor below
The scope of the present invention of shield, but it is merely representative of the selected embodiment of the present invention.Based on the embodiment in the present invention, ability
The every other embodiment that domain those of ordinary skill is obtained without creative efforts, belongs to the present invention
The range of protection.
It should be noted that：Similar label and letter represents similar terms in following attached drawing, therefore, once a certain Xiang Yi
It is defined in a attached drawing, does not then need to that it is further defined and explained in subsequent attached drawing.
In the description of the present invention, it is to be understood that the orientation or position relationship of the instructions such as term " interior ", " outer " are base
In orientation shown in the drawings or position relationship, it is for only for ease of the description present invention and simplifies description rather than instruction or imply
Signified equipment or element must have specific orientation, with specific azimuth configuration and operation, therefore it is not intended that this
The limitation of invention.
In the description of the present invention, " multiple " are meant that two or more, unless otherwise specifically defined.
In the present invention unless specifically defined or limited otherwise, term " installation ", " connected ", " connection ", " fixation " etc.
Term should be interpreted broadly, for example, it may be being fixedly connected or being detachably connected or integral；It can be direct phase
Even, it can also be indirectly connected by intermediary, can be that connection inside two elements or the interaction of two elements are closed
System.For the ordinary skill in the art, above-mentioned term in the present invention specific can be understood as the case may be
Meaning.
Embodiment of the present invention is specifically described below.
During smelting industrial silicon, impurity is contained in raw material, these impurity again silica reduction during with silicon
Element is reduced and enters industrial silicon together.In order to improve the quality of industrial silicon, the impurity content in industrial silicon is reduced, usually will
Industrial silicon carries out oxygen blast slag making in 120 to remove impurity two-maing ladle, so as to obtain the relatively low industrial silicon liquid of impurity content, then into
Row moulding by casting.But silicon liquid can slowly decline in temperature in 120 of two-maing ladle, and thermodynamic condition be caused to be deteriorated, it is impossible to when carrying out long
Between refine, many impurity can not remove.
Based on this, embodiment of the present invention provides a kind of industrial silicon rectification systems 100 and refinery practice, industrial silicon refining system
The schematic diagram of system 100 please refers to Fig. 1, and industrial silicon refinery practice figure please refers to Fig. 2.
Industrial silicon rectification systems 100 include mineral hot furnace 110, two-man ladle 120, refining furnace 130 and Temperature-controlled appliance 140, ore deposit
The discharge port of hot stove 110 is connect with 120 feed inlet of two-maing ladle, and two-maing ladle 120 is configured for carrying out silicon liquid logical oxygen reaction.
Refining furnace 130 is configured for receiving the silicon liquid after leading to oxygen reaction in 120 of two-maing ladle, 140 quilt of Temperature-controlled appliance
It is disposed for controlling the temperature in refining furnace 130.
Industrial silicon raw material is smelted in mineral hot furnace 110 to obtain silicon liquid, when the silicon liquid liquid level in mineral hot furnace 110 reaches
During certain position, artificial through-hole is carried out so that silicon liquid is flowed into from the outflow of the discharge port of mineral hot furnace 110 from 120 feed inlet of two-maing ladle
Enter to two-man ladle in 120, silicon liquid carries out the logical oxygen reaction of a period of time in 120 two-maing ladle, and it is miscellaneous to reduce iron, aluminium, calcium in silicon liquid etc.
The content of matter.By logical oxygen, treated that silicon liquid is transported to refining furnace 130, and the volume of the silicon liquid in refining furnace 130 is refining furnace
The 1/2~2/3 of 130 volumes.130 remaining volume of refining furnace can be used for follow-up addition scrap silicon and calcium class slag former.Then it is sharp
With Temperature-controlled appliance 140 to 130 feeding temperature-raising of refining furnace, add in scrap silicon and calcium class slag former is kneaded.Work as refining furnace
When 130 chargings are full, i.e. the volume of scrap silicon and calcium class slag former is the 1/3~1/2 of 130 volume of refining furnace, controls refining furnace 130
Interior temperature keeps the temperature 20~60min at 1500~1750 DEG C.Ran Hou Ru remove boiler face shoddye, and silicon liquid is poured into ready silicon packet
In, be hung to silicon ingot ingot casting area cast, silicon liquid crystallization after obtain the higher metal silicon ingot of purity, crush it is blocking after can packing and selling.
In some embodiments, refining temperature is 1600~1750 DEG C.
Wherein, scrap silicon includes polycrystalline monocrystal silicon waste materials particle, polycrystalline monocrystalline silicon Buddha's warrior attendant wire cutting briquetting material, metallic silicon
Powder and metallic silicon leftover pieces, photovoltaic battery panel give up at least one of fragment.Metallic silicon powder includes the dedusting of refining furnace 130
Powder.
The content of scrap silicon silicon selected by present embodiment is higher, and other impurities are less.What is cleaned to silicon liquid
Meanwhile and the content of silicon is increased, thus impurity is less in final silicon liquid and silicone content is high.In addition scrap silicon again can waste profit
With energy conservation and environmental protection.
It should be noted that when the scrap silicon added in is polycrystalline monocrystal silicon waste materials particle, polycrystalline monocrystalline silicon Buddha's warrior attendant wire cutting
It is negligible since its iron content, aluminium, calcium content are very low, and substantially during briquetting material.It is final can obtain national standard 3303,
2202nd, the metallic silicon of 1101 trades mark.When the scrap silicon of addition is metallic silicon powder and metallic silicon leftover pieces, national standard can obtain
421 low aluminium, low calcium metallic silicon.Wherein, the impurity content of each trade mark please refers to following table.
| The trade mark | 553 | 441 | 421 | 3303 | 2202 | 1101 |
| Iron | <0.5 | <0.4 | <0.4 | <0.3 | <0.2 | <0.1 |
| Aluminium | <0.5 | <0.4 | <0.2 | <0.3 | <0.2 | <0.1 |
| Calcium | <0.3 | <0.1 | <0.1 | <0.03 | <0.02 | <0.01 |
In the present embodiment, calcium class slag former includes at least one of calcium oxide, calcium hydroxide and calcirm-fluoride.
Calcium oxide, calcium hydroxide and calcirm-fluoride are respectively provided with preferably slag making effect, can preferably remove sulphur in silicon liquid,
The impurity such as phosphorus, carbon.
In addition, in some embodiments, refining furnace 130 is provided with multiple, and multiple refining furnaces 130 are correspondingly arranged temperature
Control device 140.
The benefit set in this way is that the silicon liquid two-mand ladle in 120 can be dispensed by multiple refining furnaces 130.In addition, this embodiment party
The refining furnace 130 of formula has the function of electromagnetic induction heating, and Temperature-controlled appliance 140 includes frequency-conversion control cabinet 141 and electric furnace transformation
Device 142 please refers to Fig. 3, and refining furnace 130 is electrically connected with the compensation capacitor of frequency-conversion control cabinet 141, frequency-conversion control cabinet 141 and electricity
Furnace transformer 142 is electrically connected, and variable alternating voltage is provided by furnace transformer 142, it is defeated that frequency-conversion control cabinet 141 plays adjusting
Go out the effect of power, so as to ensure that the temperature of refining furnace 130 is kept within a certain range.
Further, Fig. 4 is please referred to, industrial silicon rectification systems 100 further include petticoat pipe 131 and deduster 132.Petticoat pipe 131
For collecting the flue dust of refining furnace 130, petticoat pipe 131 is connect with deduster 132.Wherein, the flue dust that refining furnace 130 generates is by petticoat pipe
131 collect, and the flue dust of collection is in deduster 132 by processing dedusting.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
Raw material is smelted to obtain purity for 98% silicon liquid in mineral hot furnace 110, when the silicon liquid liquid in mineral hot furnace 110
When face reaches predeterminated position, carry out artificial through-hole so that silicon liquid from the outflow of the discharge port of mineral hot furnace 110 from two-man ladle 120 charging
Mouthful stream, which enters, two-mans ladle in 120, and silicon liquid carries out the logical oxygen reaction of 20min in 120 two-maing ladle.By logical oxygen, treated that silicon liquid pours into essence
In furnace 130, the volume of silicon liquid is the 1/2 of 130 volume of refining furnace.Then the controller of frequency-conversion control cabinet 141 is opened, to refining furnace
130 feeding temperature-raisings add in polycrystalline monocrystal silicon waste materials particle, polycrystalline monocrystalline silicon Buddha's warrior attendant wire cutting briquetting material and calcium oxide to refining
Stove 130 is full, and the temperature in refining furnace 130 is controlled to keep the temperature 60min after being kneaded at 1680 DEG C.Ran Hou Ru remove boiler face shoddye, will
Silicon liquid is poured into ready silicon packet, is hung to the cast of silicon ingot ingot casting area, the higher metal silicon ingot of purity is obtained after silicon liquid crystallization,
In, the content of iron<0.25%, the content of aluminium<0.23%, the content of calcium<0.024%.
Embodiment 2
Raw material is smelted to obtain purity for 98% silicon liquid in mineral hot furnace 110, when the silicon liquid liquid in mineral hot furnace 110
When face reaches predeterminated position, carry out artificial through-hole so that silicon liquid from the outflow of the discharge port of mineral hot furnace 110 from two-man ladle 120 charging
Mouthful stream, which enters, two-mans ladle in 120, and silicon liquid carries out the logical oxygen reaction of 20min in 120 two-maing ladle.By logical oxygen, treated that silicon liquid pours into essence
In furnace 130, the volume of silicon liquid is the 2/3 of 130 volume of refining furnace.The controller of frequency-conversion control cabinet 141 is then turned on, to refining
130 feeding temperature-raising of stove, adding in metallic silicon powder and metallic silicon leftover pieces and calcium hydroxide to refining furnace 130 expires, and controls refining furnace
Temperature in 130 keeps the temperature 60min after being kneaded at 1500 DEG C.Ran Hou Ru remove boiler face shoddye, and silicon liquid is poured into ready silicon
Bao Zhong is hung to the cast of silicon ingot ingot casting area, the higher metal silicon ingot of purity is obtained after silicon liquid crystallization, wherein, the content of iron<
0.33%, the content of aluminium<0.15%, the content of calcium<0.05%.
Embodiment 3
Raw material is smelted to obtain purity for 98% silicon liquid in mineral hot furnace 110, when the silicon liquid liquid in mineral hot furnace 110
When face reaches predeterminated position, carry out artificial through-hole so that silicon liquid from the outflow of the discharge port of mineral hot furnace 110 from two-man ladle 120 charging
Mouthful stream, which enters, two-mans ladle in 120, and silicon liquid carries out the logical oxygen reaction of 20min in 120 two-maing ladle.By logical oxygen, treated that silicon liquid pours into essence
In furnace 130, the volume of silicon liquid is the 2/3 of 130 volume of refining furnace.The controller of frequency-conversion control cabinet 141 is then turned on, to refining
130 feeding temperature-raising of stove, adding in metallic silicon powder and polycrystalline monocrystal silicon waste materials particle and calcirm-fluoride to refining furnace 130 expires, control essence
Temperature in furnace 130 keeps the temperature 20min after being kneaded at 1750 DEG C.Ran Hou Ru remove boiler face shoddye, and silicon liquid is poured into and is ready to
Silicon packet in, be hung to silicon ingot ingot casting area cast, silicon liquid crystallization after obtain the higher metal silicon ingot of purity, wherein, the content of iron<
0.33%, the content of aluminium<0.21%, the content of calcium<0.08%.
The foregoing is merely the preferred embodiment of the present invention, are not intended to restrict the invention, for this field
For technical staff, the invention may be variously modified and varied.All within the spirits and principles of the present invention, that is made is any
Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of industrial silicon rectification systems, which is characterized in that it includes：Mineral hot furnace is two-mand ladle, refining furnace and Temperature-controlled appliance,
The discharge port of the mineral hot furnace is connect with the feed inlet two-mand ladle, it is described two-man ladle be configured for carrying out silicon liquid logical oxygen it is anti-
It should；
The refining furnace is two-mand ladle the silicon liquid after interior logical oxygen reaction described in being configured for receiving, the Temperature-controlled appliance
It is configured for controlling the temperature in the refining furnace.
2. industrial silicon rectification systems according to claim 1, which is characterized in that the refining furnace be provided with it is multiple, it is multiple
The refining furnace is correspondingly arranged the Temperature-controlled appliance.
3. industrial silicon rectification systems according to claim 1 or 2, which is characterized in that the industrial silicon rectification systems also wrap
Petticoat pipe and deduster are included, the petticoat pipe is used to collect the flue dust of the refining furnace, and the petticoat pipe is connect with the deduster.
4. a kind of industrial silicon refinery practice, which is characterized in that it mainly utilizes claim 1-3 any one of them industrial silicon essence
Refining system carries out, including：Industrial silicon raw material is smelted in the mineral hot furnace to obtain silicon liquid, by the silicon in the mineral hot furnace
Liquid be discharged into it is described two-man ladle it is interior carry out logical oxygen reaction, the silicon liquid after leading to oxygen reaction is discharged into the refining furnace, the refining furnace
The volume of the interior silicon liquid for the refining furnace volume 1/2~2/3, using the Temperature-controlled appliance by the refining furnace
Interior temperature is controlled at 1500~1750 DEG C, then adds in scrap silicon and calcium class slag former is kneaded and is kept the temperature, described in removal
Shoddye in refining furnace obtains purer silicon liquid.
5. industrial silicon refinery practice according to claim 4, which is characterized in that the scrap silicon gives up including polycrystalline monocrystalline silicon
Material particle, polycrystalline monocrystalline silicon Buddha's warrior attendant wire cutting briquetting material, metallic silicon powder and metallic silicon leftover pieces, photovoltaic battery panel give up fragment
At least one of.
6. industrial silicon refinery practice according to claim 5, which is characterized in that the metallic silicon powder includes metallic silicon system
Dust-removing powder in powder or crushing process.
7. industrial silicon refinery practice according to claim 4, which is characterized in that the calcium class slag former include calcium oxide,
At least one of calcium hydroxide and calcirm-fluoride.
8. industrial silicon refinery practice according to claim 4, which is characterized in that the temperature of the refining is 1600~1750
℃。
9. industrial silicon refinery practice according to claim 4, which is characterized in that the soaking time of the silicon liquid for 20~
60min。
10. industrial silicon refinery practice according to claim 4, which is characterized in that the scrap silicon and the calcium class slag making
The volume of agent refines the 1/3~1/2 of furnace volume to be described.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110332806A (en) * | 2019-07-05 | 2019-10-15 | 国工恒昌新材料沧州有限公司 | A kind of exotic metal alloys material Refining device and its application method |
| CN111270095A (en) * | 2020-03-30 | 2020-06-12 | 邱清余 | Refining system and process for refining aluminum-based alloy by hot mixing of molten aluminum and molten silicon |
| CN111807372A (en) * | 2020-07-21 | 2020-10-23 | 昆明理工大学 | Method for top-blown refining of silicon wafer cutting waste |
| CN114212795A (en) * | 2021-12-21 | 2022-03-22 | 湖南立新硅材料科技有限公司 | Device and method for refining silicon sludge |
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