CN104909368B - The method for processing silicon liquid - Google Patents
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- CN104909368B CN104909368B CN201510274005.8A CN201510274005A CN104909368B CN 104909368 B CN104909368 B CN 104909368B CN 201510274005 A CN201510274005 A CN 201510274005A CN 104909368 B CN104909368 B CN 104909368B
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Abstract
The invention provides a kind of method for processing silicon liquid, contains aluminum, calcium, phosphorus and boron in the silicon liquid, methods described includes：(1) using silicon liquid described in dioxygen oxidation, and refining agent and slag former are added in the silicon liquid, to obtain solid oxidation slag and silicon melt containing aluminium sesquioxide, calcium oxide and silicon dioxide；(2) the solid oxidation slag containing aluminium sesquioxide, calcium oxide and silicon dioxide and silicon melt are separated, to respectively obtain solid oxidation slag and silicon melt containing aluminium sesquioxide, calcium oxide and silicon dioxide.The method can significantly improve the clearance of aluminum, calcium, phosphorus and boron impurity in silicon liquid, and the response rate of element silicon can reach 86% in the silicon melt for obtaining.
Description
Technical field
The invention belongs to non-ferrous metal metallurgy technical field, specifically, the present invention relates to a kind of method for processing silicon liquid.
Background technology
The silicon liquid containing impurity for producing in domestic industry silicon production technology at present is generally aoxidized using traditional extensive style
Method of refining.In actual applications, refining time is long for this method of refining, and silicon loss rate is big, and division operation is inconvenient outer, is formed
Tailings be difficult again to separate with silicon melt so that the degree of purity of silicon liquid is difficult to improve, thus contain in the tailings for being formed
The silicon of considerable quantity, causes the loss of silicon resource, and causes unit of the product consumption and cost to increase；Simultaneously because to P,
The trace element management and control such as B is not in place so that the silicon melt of gained cannot fully meet the production requirements such as metallic silicon downstream industry chain.
Therefore, the existing technology for processing silicon liquid is further improved.
The content of the invention
It is contemplated that at least solving one of technical problem in correlation technique to a certain extent.For this purpose, the present invention
One purpose is to propose a kind of method for processing silicon liquid, and the method can significantly improve aluminum, calcium, phosphorus and boron impurity in silicon liquid
In clearance, and the silicon melt for obtaining, the response rate of element silicon can reach 86%.
In one aspect of the invention, the present invention propose it is a kind of process silicon liquid method, in the silicon liquid containing aluminum,
Calcium, phosphorus and boron, methods described include：
(1) using silicon liquid described in dioxygen oxidation, and refining agent and slag former are added in the silicon liquid, to be contained
The solid oxidation slag of aluminium sesquioxide, calcium oxide and silicon dioxide and silicon melt；And
(2) the solid oxidation slag containing aluminium sesquioxide, calcium oxide and silicon dioxide and silicon melt are carried out point
From to respectively obtain solid oxidation slag and silicon melt containing aluminium sesquioxide, calcium oxide and silicon dioxide.
Thus, the method for process silicon liquid according to embodiments of the present invention can significantly improve going for aluminum, calcium, phosphorus and boron impurity
Except efficiency, and the response rate of element silicon can reach 86% in the silicon melt for obtaining, such that it is able to be prevented effectively from silicon resource
Waste.
In addition, the method for processing silicon liquid according to the above embodiment of the present invention can also have following additional technology special
Levy：
In some embodiments of the invention, step (1) is carried out according to the following steps：(1-1) silicon liquid is supplied
To into two-maing ladle, and oxygen is supplied from the bottom of two-maing ladle in the silicon liquid；(1-2) in the silicon liquid obtained to step (1-1)
Refining agent is added, and gained mixing silicon liquid is heated；And (1-3) will be added and be made in mixing silicon liquid obtained by step (1-2)
Slag agent, to obtain the solid oxidation slag containing aluminium sesquioxide, calcium oxide and silicon dioxide and silicon melt.Thus,
The response rate of element silicon can further be improved.
In some embodiments of the invention, in step (1-2), the addition of the refining agent is the silicon liquid quality
0.5%～3%.Thus, it is possible to further improve the response rate of element silicon.
In some embodiments of the invention, the refining agent is selected from calcium oxide, aluminium oxide, magnesium oxide, sodium oxide, oxygen
Change at least one in potassium, calcium fluoride and calcium chloride.Thus, it is possible to further improve the response rate of element silicon.
In some embodiments of the invention, in step (1-2), the mixing silicon liquid is heated to into 1450～1550 and is taken the photograph
Family name's degree.Thus, it is possible to further improve the response rate of element silicon.
In some embodiments of the invention, in step (1-3), the addition of the slag former is the silicon liquid quality
0.5～3%.Thus, it is possible to effectively improve the molten of the solid oxidation slag containing aluminium sesquioxide, calcium oxide and silicon dioxide
Point, so as to the response rate for improving element silicon while the removal efficiency of aluminum, calcium, phosphorus and boron impurity is improved.
In some embodiments of the invention, the slag former contains Calcium Carbonate, magnesium sulfate and Zinc Oxide.Thus, it is possible to
The response rate of element silicon is improved further.
In some embodiments of the invention, the slag former contains the Calcium Carbonate of 30～40wt%, 20～30wt%
The Zinc Oxide of magnesium sulfate and 30～40wt%.Thus, it is possible to further improve the response rate of element silicon.
In some embodiments of the invention, the response time of step (1) is 15～120min.Thus, it is possible to further
Improve the response rate of element silicon.
In some embodiments of the invention, in the silicon liquid, silicone content is more than 95wt%.
The additional aspect and advantage of the present invention will be set forth in part in the description, and partly will become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Description of the drawings
The above-mentioned and/or additional aspect and advantage of the present invention will become from the description with reference to accompanying drawings below to embodiment
It is substantially and easy to understand, wherein：
Fig. 1 is the method flow schematic diagram for processing silicon liquid according to an embodiment of the invention；
Fig. 2 is the method flow schematic diagram of the process silicon liquid according to another embodiment of the invention.
Specific embodiment
Embodiments of the invention are described below in detail, the example of the embodiment is shown in the drawings, wherein from start to finish
Same or similar label represents same or similar element or the element with same or like function.Below with reference to attached
The embodiment of figure description is exemplary, it is intended to for explaining the present invention, and be not considered as limiting the invention.
In one aspect of the invention, the present invention proposes a kind of method for processing silicon liquid.Embodiments in accordance with the present invention,
Contain aluminum, calcium, phosphorus and boron in silicon liquid.Embodiments in accordance with the present invention, the method include：(1) using dioxygen oxidation silicon liquid, and to
Refining agent and slag former are added in silicon liquid, to obtain the solid oxidation slag containing aluminium sesquioxide, calcium oxide and silicon dioxide
And silicon melt；And the solid oxidation slag containing aluminium sesquioxide, calcium oxide and silicon dioxide and silicon melt are carried out by (2)
Separate, to respectively obtain solid oxidation slag and silicon melt containing aluminium sesquioxide, calcium oxide and silicon dioxide.Inventor
It was found that, by the impurity aluminum in silicon liquid, calcium, phosphorus and boron and a small amount of silica being turned to oxidation using dioxygen oxidation silicon liquid
Thing, wherein the phosphorus pentoxide for generating and boron oxide are removed in the form of volatilizing, and generate aluminium sesquioxide, calcium oxide and
Silicon dioxide is as fusing point is higher than the fusing point of silicon melt so that aluminium sesquioxide, calcium oxide and silicon dioxide are with solid oxidation slag
Form is present, and so as to utilize the two different melting points to be separated, and adds fusing point to carry out refine higher than the refining agent of silicon,
Foreign ion can be caused to be enriched in oxidizing slag, can be realized that oxidizing slag and silicon melt are sufficiently separated so as to pass through cooling, be entered
And the grade of raising silicon melt, while the fusing point of solid oxidation slag by slag former is added in silicon liquid, can be significantly improved, from
And be prevented effectively from substantial amounts of solid oxidation slag and redissolve in silicon melt, and then the removal efficiency of aluminum and calcium impurities is significantly improved, and
And in silicon liquid add slag former significantly improve the volatilization efficiency of phosphorus pentoxide and boron oxide, so as to further improve silicon
Impurity removal efficacy in liquid, and then the response rate of the grade and silicon of silicon in silicon melt is significantly improved, in addition, the method operation letter
It is single, it is with low cost, it is not necessary to extra equipment investment.
The method of the process silicon liquid of the embodiment of the present invention is described in detail below with reference to Fig. 1.Reality of the invention
Example is applied, the method includes：
S100：Using dioxygen oxidation silicon liquid, and refining agent and slag former are added in silicon liquid
Embodiments in accordance with the present invention, using dioxygen oxidation silicon liquid, and add refining agent and slag former in silicon liquid, so as to
Solid oxidation slag and silicon melt containing aluminium sesquioxide, calcium oxide and silicon dioxide can be obtained.Inventor has found, utilizes
Dioxygen oxidation silicon liquid, due to the difference of silicon and the chemical property of aluminum, calcium, phosphorus and boron, can cause most aluminum, calcium, phosphorus and
Boron is oxidized to corresponding oxide, while a small amount of silicon is oxidized to silicon dioxide, and the part of silica can be by silicon
Impurity aluminum and calcium reduction in liquid is elementary silicon, hence in so that only a small amount of silicon is in the form of silicon dioxide, so as to can
The waste of silicon resource is caused to be prevented effectively from substantial amounts of silicon in solid oxidation slag, wherein, phosphorus and boron element can be respectively
The volatilization in the form of phosphorus pentoxide and boron oxide is removed, and due to the fusing point of aluminium sesquioxide, calcium oxide, silicon dioxide and silicon
Difference, can cause aluminium sesquioxide, calcium oxide and silicon dioxide in the form of solid oxidation slag, and silicon is with melt form
Exist, and add fusing point refine to be carried out higher than the refining agent of silicon, foreign ion can be caused to be enriched in oxidizing slag, so as to logical
Cross cooling and can realize that oxidizing slag and silicon melt are sufficiently separated, and then improve the grade of silicon melt, while by adding in silicon liquid
Enter slag former, the fusing point of solid oxidation slag can be significantly improved, it is poor so as to improve the fusing point between solid oxidation slag and silicon melt, enter
And be prevented effectively from substantial amounts of solid oxidation slag and redissolve in silicon melt, and then the removal efficiency of aluminum and calcium impurities is significantly improved, and
And in silicon liquid add slag former significantly improve the volatilization efficiency of phosphorus pentoxide and boron oxide, so as to further improve silicon
Impurity removal efficacy in liquid, and then significantly improve the response rate of the grade and silicon of silicon in silicon melt.
With reference to Fig. 2, embodiments in accordance with the present invention, S100 steps can be carried out according to the following steps：
S110：Silicon liquid is supplied into two-maing ladle, and supplies oxygen from bottom of two-maing ladle in silicon liquid
Embodiments in accordance with the present invention, silicon liquid is supplied into two-maing ladle, and supplies oxygen from bottom of two-maing ladle in silicon liquid, from
And most aluminum, calcium, phosphorus and boron are oxidized to corresponding oxide in can causing silicon liquid, while a small amount of silicon is oxidized to
Silicon dioxide, and the part of silica can be elementary silicon by the impurity aluminum and calcium reduction in silicon liquid, hence in so that only few
The silicon of amount causes silicon to provide such that it is able to be prevented effectively from substantial amounts of silicon in solid oxidation slag in the form of silicon dioxide
The waste in source, wherein the phosphorus pentoxide for generating and boron oxide are removed in the form of volatilizing.In the step, specifically, first
By the silicon content released in mineral hot furnace more than 95% silicon liquid enter can be with oxygen blown two-maing ladle to bottom in, wherein, in silicon liquid not
When inflow two-mans ladle middle, by the bottom oxygen intake compressed air that middle supply flow rate is 300L/min to two-maing ladle of two-maing ladle, and ensure
Trachea is unimpeded, after silicon liquid is flowed into two-mans ladle, cuts off compressed air, by oxygen intake to middle supply flow rate of two-maing ladle for 600L/min
Oxygen.
S120：Refining agent is added in the silicon liquid obtained to S110, and gained mixing silicon liquid is heated
Embodiments in accordance with the present invention, add refining agent in silicon liquid obtained above, and gained silicon liquid are heated.
Embodiments in accordance with the present invention, the particular type of refining agent are not particularly restricted, and those skilled in the art can be according to reality
Needs are selected, and according to one embodiment of present invention, refining agent can be calcium oxide.Inventor has found, molten by adding
Point carries out refine higher than the refining agent of silicon, foreign ion can be caused to be enriched in oxidizing slag, can be realized so as to pass through cooling
Oxidizing slag and silicon melt are sufficiently separated, and then improve the grade of silicon melt.Embodiments in accordance with the present invention, the addition of refining agent
It is not particularly restricted, those skilled in the art can be selected according to actual needs, according to one embodiment of present invention, refine
The addition of agent can be the 0.5-3wt% of silicon liquid quality.Inventor has found, if refining agent addition is too high or too low all easily making
Density into the density and ternary slag of metallic silicon gets too close to, so as to cause melt silicon be separated with oxidizing slag.Thus,
Sediment can be promoted using the addition of the scope of the invention, so that silicon melt is sufficiently separated with oxidizing slag, and then silicon is improved
The grade of melt.Mixing silicon liquid can be heated to 1450～1550 degrees Celsius in the step by embodiments in accordance with the present invention.Send out
A person of good sense has been surprisingly found that by many experiments impurity element has higher oxidation reaction in not only can ensureing silicon liquid at this temperature
With reduction reaction efficiency, and can ensure that oxidizing slag is present in solid form, so as to while treatment effeciency is significantly improved
The removal efficiency of impurity element is improved, and then improves the grade of silicon in silicon melt.In the step, specifically, wait middle silicon liquid of two-maing ladle
After reaching certain mass, refining agent is added in silicon liquid, temperature control is carried out with rice straw mulching, and silicon liquid is measured using digital display temperature measurer
Temperature, control silicon liquid temperature at 1450～1550 degrees Celsius.
S130：Slag former is added by mixing in silicon liquid obtained by S120
Embodiments in accordance with the present invention, add slag former, in above-mentioned gained mixing silicon liquid such that it is able to obtain containing three
The solid oxidation slag of Al 2 O, calcium oxide and silicon dioxide and silicon melt.Thus, by adding slag making in mixing silicon liquid
Agent, can significantly improve the fusing point of solid oxidation slag, poor so as to improve the fusing point between solid oxidation slag and silicon melt, and then effectively
Avoid substantial amounts of solid oxidation slag from redissolving in silicon melt, and then significantly improve the removal efficiency of aluminum and calcium impurities, and to silicon
Add slag former significantly improve the volatilization efficiency of phosphorus pentoxide and boron oxide in liquid.Embodiments in accordance with the present invention, make
The addition of slag agent is not particularly restricted, and those skilled in the art can be selected according to actual needs, according to the present invention
One embodiment, the addition of slag former can be the 0.5～3% of silicon liquid quality.Inventor has found, using the scope of the invention
Addition can promote sediment so that silicon melt is sufficiently separated with oxidizing slag, and then further improve the product of silicon melt
Position.Embodiments in accordance with the present invention, the composition of slag former according to actual needs may not be used by particular type, those skilled in the art
Be selected to improve solid oxidation slag fusing point and will not in silicon liquid introduce impurity any kind of slag former, according to this
One embodiment of invention, slag former can contain Calcium Carbonate, magnesium sulfate and Zinc Oxide.Inventor has found, adopts and contain carbonic acid
The slag former of calcium, magnesium sulfate and Zinc Oxide, as Calcium Carbonate, magnesium sulfate and Zinc Oxide can occur chemistry with the impurity in silicon melt
Reaction, forms the slag phases different from metallic silicon fluid density, viscosity, and floats to silicon melt surface or sink to silicon melt bottom
Portion such that it is able to promote slag to separate with silicon, and silicon liquid body will not be polluted.Embodiments in accordance with the present invention, slag former
Middle each component content is not particularly restricted, and those skilled in the art can be selected according to actual needs, according to the present invention
One embodiment, slag former can the Calcium Carbonate containing 30～40wt%, the magnesium sulfate of 20～30wt% and 30～40wt%
Zinc Oxide.Inventor's discovery, can remarkably promote the separation of the foreign ion in silicon melt using the slag former of the composition, from
And further improve the grade of silicon melt.
Embodiments in accordance with the present invention, the response time of step S100 can be 15～120min.Thus, reducing production
The removal efficiency of impurity element is improved while cost further.Embodiments in accordance with the present invention, in silicon liquid, silicone content can be big
In 95%.
S200：Solid oxidation slag containing aluminium sesquioxide, calcium oxide and silicon dioxide and silicon melt are separated
Embodiments in accordance with the present invention, by the solid oxidation slag containing aluminium sesquioxide, calcium oxide and silicon dioxide and
Silicon melt is separated, such that it is able to respectively obtain the solid oxidation slag containing aluminium sesquioxide, calcium oxide and silicon dioxide with
And silicon melt.Embodiments in accordance with the present invention, the solid oxidation slag containing aluminium sesquioxide, calcium oxide and silicon dioxide and silicon
The separate mode of melt is not particularly restricted, and those skilled in the art can be selected according to actual needs, according to this
Solid oxidation slag of the gained containing aluminium sesquioxide, calcium oxide and silicon dioxide and silicon can be melted by bright one embodiment
Mop that the mixture of body is poured into during ingot mould on by two-maing ladle so that solid oxidation slag stays in and two-mans ladle in, then manually enter
Row removing is processed, and the silicon melt for obtaining can carry out break process and obtain finished product after cooling down.
Below with reference to specific embodiment, present invention is described, it should be noted that these embodiments are only described
Property, and the present invention is limited never in any form.
Embodiment
Silicon liquid first by the silicon content released in mineral hot furnace more than 95% is entered can be with oxygen blown two-maing ladle to bottom, its
In, when in silicon liquid not flowed into and two-mand ladle, by the bottom oxygen intake compression that middle supply flow rate is 300L/min to two-maing ladle of two-maing ladle
Air, and ensure that trachea is unimpeded, after silicon liquid is flowed into two-mans ladle, compressed air is cut off, by oxygen intake to middle supply stream of two-maing ladle
The oxygen for 600L/min is measured, then after middle silicon liquid of two-maing ladle reaches 5000kg, 45-150kg calcium oxide essence is added in silicon liquid
Refining agent, carries out temperature control with rice straw mulching, and the temperature of silicon liquid is measured using digital display temperature measurer, control silicon liquid temperature 1450～
1550 degrees Celsius, then to gained mix silicon liquid in add 30～100kg slag former (Calcium Carbonate containing 30～40wt%,
The Zinc Oxide of the magnesium sulfate and 30～40wt% of 20～30wt%), such that it is able to obtain containing aluminium sesquioxide, calcium oxide and two
The solid oxidation slag and the mixture of silicon melt of silicon oxide, finally by containing aluminium sesquioxide, calcium oxide and silicon dioxide
The mop that the mixture of solid oxidation slag and silicon melt is poured into during ingot mould on by two-maing ladle is so that solid oxidation slag is stayed
In two-maing ladle, process is then manually purged, and the silicon melt for obtaining can carry out break process and obtain finished product after cooling down.With
The elevated raising of temperature, the removal efficiency of impurity increases, and at 1500 DEG C, Ca basically reaches the maximum of removing, 1460
DEG C when, Al reaches the removal efficiency of maximum, and knowable to being detected to gained silicon melt, in silicon liquid Al extrusion rates reach 80% with
On, Ca extrusion rates reach more than 95%, and the extrusion rate such as P, B brings up to more than 75%, and the silicon response rate reaches 86%, so that silicon
Melt can fully meet the production requirements such as metallic silicon downstream industry chain.
Wherein, silicon melt per ton is produced, the consumption of refining agent calcium oxide is less than 13m less than 14kg, air consumption3, mark coal disappear
Consumption is less than 0.090 ton, it is possible thereby to significantly reduce smelting industrial silicon energy consumption and processing cost.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
Example ", or the description of " some examples " etc. mean specific features with reference to the embodiment or example description, structure, material or spy
Point is contained at least one embodiment or example of the present invention.In this manual, to the schematic representation of above-mentioned term not
Identical embodiment or example must be directed to.And, the specific features of description, structure, material or feature can be with office
Combined in one or more embodiments or example in an appropriate manner.Additionally, in the case of not conflicting, the skill of this area
The feature of the different embodiments or example described in this specification and different embodiments or example can be tied by art personnel
Close and combine.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changes, replacing and modification.
Claims (6)
1. a kind of method for processing silicon liquid, contains aluminum, calcium, phosphorus and boron, it is characterised in that methods described includes in the silicon liquid：
(1) using silicon liquid described in dioxygen oxidation, and refining agent and slag former are added in the silicon liquid, to obtain containing three oxygen
Change the solid oxidation slag and silicon melt of two aluminum, calcium oxide and silicon dioxide；And
(2) the solid oxidation slag containing aluminium sesquioxide, calcium oxide and silicon dioxide and silicon melt are separated, with
Just solid oxidation slag and silicon melt containing aluminium sesquioxide, calcium oxide and silicon dioxide are respectively obtained,
Wherein, step (1) is carried out according to the following steps：
(1-1) silicon liquid is supplied into two-maing ladle, and supplies oxygen from the bottom of two-maing ladle in the silicon liquid；
(1-2) refining agent is added in the silicon liquid obtained to step (1-1), and gained mixing silicon liquid is heated；And (1-3)
Slag former is added by mixing in silicon liquid obtained by step (1-2), it is described containing aluminium sesquioxide, calcium oxide and titanium dioxide to obtain
The solid oxidation slag of silicon and silicon melt,
In step (1-3), the addition of the slag former is the 0.5-3% of the silicon liquid quality,
The slag former contains the Zinc Oxide of the Calcium Carbonate of 30～40wt%, the magnesium sulfate of 20～30wt% and 30～40wt%.
2. method according to claim 1, it is characterised in that in step (1-2), the addition of the refining agent is institute
State the 0.5%～3% of silicon liquid quality.
3. method according to claim 2, it is characterised in that the refining agent is selected from calcium oxide, aluminium oxide, oxidation
At least one in magnesium, sodium oxide, potassium oxide, calcium fluoride and calcium chloride.
4. method according to claim 1, it is characterised in that in step (1-2), the mixing silicon liquid is heated to
1450～1550 degrees Celsius.
5. method according to claim 1, it is characterised in that the response time of step (1) is 15～120min.
6. method according to claim 1, it is characterised in that silicone content is more than 95wt% in the silicon liquid.
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| CN105329901B (en) * | 2015-10-22 | 2017-10-27 | 昆明理工大学 | It is a kind of that the method that zinc compound removes boron impurity in industrial silicon is added into calcium silicates |
| CN111807372B (en) * | 2020-07-21 | 2022-08-26 | 昆明理工大学 | Method for top-blown refining of silicon wafer cutting waste |
| CN114644339B (en) * | 2022-04-29 | 2023-04-25 | 成都理工大学 | Method for removing impurities in silicon by adopting inorganic zinc salt |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101712474A (en) * | 2009-09-08 | 2010-05-26 | 南安市三晶阳光电力有限公司 | Method for preparing solar-grade high-purity silicon by dilution purifying technology |
| CN101774584A (en) * | 2009-01-09 | 2010-07-14 | 华南师范大学 | Method for purifying solar-grade silicon |
| CN102583389A (en) * | 2012-03-05 | 2012-07-18 | 昆明理工大学 | Method for purifying industrial silicon through external refining |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774584A (en) * | 2009-01-09 | 2010-07-14 | 华南师范大学 | Method for purifying solar-grade silicon |
| CN101712474A (en) * | 2009-09-08 | 2010-05-26 | 南安市三晶阳光电力有限公司 | Method for preparing solar-grade high-purity silicon by dilution purifying technology |
| CN102583389A (en) * | 2012-03-05 | 2012-07-18 | 昆明理工大学 | Method for purifying industrial silicon through external refining |
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