CN105110337A - Method for deep impurity removal in metallic silicon smelting - Google Patents
Method for deep impurity removal in metallic silicon smelting Download PDFInfo
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Abstract
The invention belongs to the field of metallic silicon smelting technologies, and particularly relates to a method for deep impurity removal in metallic silicon smelting. The method comprises six steps, namely, preparation of a combined flocculating agent, high-temperature melting, oxygen blowing for refinement, sampling for detection, deep aluminum removal and filtration for impurity removal. With the adoption of the method, the content of aluminum in metallic silicon can be reduced and controlled within 0.18% in a traditional refining process, metallurgical grade silicon can be improved to chemical grade silicon under the condition that refining procedures are not increased excessively, the effect is better, and the cost is low.
Description
Technical field
The invention belongs to metallic silicon smelting technology field, be specifically related to a kind of method of metallic silicon smelting deep impurity-removing.
Background technology
The requirement of Pure Silicon Metal to impurity Fe, Al, Ca etc. especially is wherein very high.In silicon metal smelting process, oxygen blast refining can reach about 93% to the clearance of calcium, and is only 68% ~ 80% to the clearance of aluminium.Owing to continuing the different purposes requirements of product, in recent years, market requires more and more higher to the quality of Pure Silicon Metal product, kind, in production practice, how improve the quality of products expansion range of product, is the problem that each manufacturer must pay close attention to, and is also the inevitable behave strengthening market competitiveness of enterprises, meanwhile, the important channel of Business Economic Benefit is improved especially.
In the production of traditional Pure Silicon Metal, improve Pure Silicon Metal quality product, expand mainly passing through " cleaning raw material " (namely adopting clean mineral products and high-quality reductive agent), strengthening refining or removing target impurity with acid after melting recrystallization thus obtain more high-grade silicon of range of product.This kind of improve the quality of products expand range of product technique means in, " cleaning raw material " mode is limited by that high grade raw material resources is limited and price is high, and strengthening refining route is unfavorable for saving energy and reduce the cost, the mode of purifying with acid then technique relative complex, dangerous.Therefore, developing new refinery practice or study new Impurity removal means, is a kind of new trend improving Pure Silicon Metal quality product, expand range of product.
Summary of the invention
For solving above technology Problems existing, the invention provides a kind of method of metallic silicon smelting deep impurity-removing, effectively can reduce the content of impurity aluminum in Pure Silicon Metal, promote the quality of Pure Silicon Metal.
Its technical scheme is:
A method for metallic silicon smelting deep impurity-removing, carry out according to following steps:
(1) combination wadding agent configuration: magnesium salts and sodium salt are mixed into according to a certain percentage the agent of combination wadding for subsequent use;
(2) high temperature melting: being dropped in smelting furnace by the silicon ore containing impurity, is melt under the environment of 1700 DEG C ~ 1800 DEG C in temperature;
(3) oxygen blast refining: keep the temperature in smelting furnace to remain on 1600 DEG C ~ 1700 DEG C, the oxygen of abundance is passed in silicon water;
(4) sampling detects: keep the temperature in smelting furnace to remain on 1600 DEG C ~ 1650 DEG C, waits when being refined to a certain degree, sampling analysis aluminium content (have experience person also can visual inspection);
(5) degree of depth is except aluminium: if in silicon water during aluminium content >=11%, open fire door and release silicon water, when silicon water flows to silicon bag three/start to drop into 1/3rd of ready combination dealumination agent total amount for the moment, silicon water drops into 1/3rd of ready combination dealumination agent total amount again when flowing to silicon bag 2/3rds, silicon water drops into 1/3rd of ready combination dealumination agent total amount again when flowing to silicon bag 4/5ths, keep silicon water temp at about 1650 DEG C in the process that feeds intake, and need to complete in 30 minutes.
(6) filtering and impurity removing: by the degree of depth except the slag removing in the silicon water after aluminium.
Further, in the agent of described step (1) combination wadding, the outfit ratio of magnesium salts and sodium salt is different and different according to aluminium content in silicon water, specifically carries out as follows:
(1) when aluminium content is between 11% ~ 19%, Gui Shui ﹕ Mei Yan ﹕ sodium salt=2500 ﹕ 14 ﹕ 30;
(2) when aluminium content is between 20% ~ 0.30%, Gui Shui ﹕ Mei Yan ﹕ sodium salt=2500 ﹕ 21 ﹕ 30;
(3) when in silicon water, aluminium content is more than 30%, Gui Shui ﹕ Mei Yan ﹕ sodium salt=2500 ﹕ 40 ﹕ 57.
Further, described magnesium salts is magnesium chloride, and sodium salt is sodium carbonate.
In silicon metal smelting process, the impurity in starting material, as ferric oxide, aluminium sesquioxide, calcium oxide etc., is melting in silicon water together after reduction under the high temperature conditions, is formed alloy with silicon.Silicon water normally come out of the stove be temperature at about 1800 DEG C, temperature during oxygen blast refining is greatly about 1600 DEG C to 1700 DEG C.Aluminium in the oxygen be now filled with and silicon water, calcium reflect and generate slag, and the main component of slag is aluminium sesquioxide, calcium oxide.By testing silicon water sampling, the avidity of oxygen-calcium is stronger than the avidity of oxygen-aluminium, and after being filled with oxygen, in silicon, the clearance of calcium can reach 93%, but the clearance of aluminium is only 68-80%.So also need to carry out the degree of depth except aluminium, the agent of combination wadding is added as dealumination agent in liquid-state silicon, effectively can improve the avidity of aluminium and oxygen, change it active, thus the degree of depth on original basis of the aluminium element in Pure Silicon Metal is removed, reach the requirement that low aluminum i ndustry silicon product standard is produced in dealuminzation purification, and silicon can also be made to be separated completely with slag, thus improve the yield of product, be conducive to finishing.Wherein, dealumination agent Main Function is to provide sodium, magnesium ion, in order to improve the activity of aluminium element in liquid-state silicon, changes the avidity of aluminium element and oxygen, promote that the reaction of oxygen and aluminium generates slag or sodium, magnesium ion and aluminium generate alloy crystallization, thus a large amount of aluminium content reduced in silicon water.By dealumination agent, the density of slag is reduced, change its viscosity and surface tension, make slag swim in silicon water surface, be conducive to slag and be separated with silicon.
Beneficial effect of the present invention:
(1) the present invention is applicable to the not high ore deposit product of the degree of cleaning such as high alumina silicon ore deposit, and can not cause the silicon deterioration in quality of smelting out, expands raw-material source, be conducive to reducing costs, improving data using rate in Pure Silicon Metal production practice.
(2) adopt the present invention the aluminium content in Pure Silicon Metal can be fallen control in conventional refining processes within 0.18%, metallurgical grade silicon can be made to rise to the grade of chemical grade silicon when exceeding and increasing refining procedures, effectiveness comparison is good, cost is low.
(3) the present invention does not absorb water in atmosphere at the combination dealumination agent of configuration, does not make moist, about a week can be placed, during interpolation, silicon water and surperficial slag can not splash, operate fairly simple, safety, and addition is few, price is low, silicon per ton spends combination wadding agent price at about 30 yuan, very cheap.
(4) the combination wadding agent of the present invention's use, effectively can improve avidity and the activity of aluminium and oxygen, thus the degree of depth on original basis of the aluminium element in silicon is removed, reach the requirement of low aluminium product standard, and the proportion of slag, viscosity and surface tension can also be changed, promote that silicon is separated completely with slag, thus improve the yield of product, be conducive to finishing.
Embodiment
A kind of method of metallic silicon smelting deep impurity-removing.
Example 1
Carry out according to following steps:
(1) combination wadding agent configuration: magnesium chloride and sodium carbonate are mixed into according to a certain percentage the agent of combination wadding for subsequent use;
(2) high temperature melting: being dropped in smelting furnace by the silicon ore containing impurity, is melt under the environment of 1700 DEG C ~ 1800 DEG C in temperature;
(3) oxygen blast refining: keep the temperature in smelting furnace to remain on 1600 DEG C ~ 1700 DEG C, the oxygen of abundance is passed in silicon water;
(4) sampling detects: keep the temperature in smelting furnace to remain on 1600 DEG C ~ 1650 DEG C, waits when being refined to a certain degree, sampling analysis aluminium content;
(5) degree of depth is except aluminium: detect through sampling, in silicon water, aluminium content is between 11% ~ 19%, and the wad a quilt with cotton ratio of agent of the combination in described silicon water and step (1) is Gui Shui ﹕ Lvization Mei ﹕ sodium carbonate=2500 ﹕ 14 ﹕ 30; Open fire door and release silicon water, when silicon water flows to silicon bag three/start to drop into 1/3rd of ready combination dealumination agent total amount for the moment, silicon water drops into 1/3rd of ready combination dealumination agent total amount again when flowing to silicon bag 2/3rds, silicon water drops into 1/3rd of ready combination dealumination agent total amount again when flowing to silicon bag 4/5ths, keep silicon water temp at about 1650 DEG C in the process that feeds intake, and need to complete in 30 minutes.
(6) filtering and impurity removing: by the degree of depth except the slag removing in the silicon water after aluminium, in the silicon water of gained, aluminium content is 0.16%.
Example 2
Carry out according to following steps:
(1) combination wadding agent configuration: magnesium chloride and sodium carbonate are mixed into according to a certain percentage the agent of combination wadding for subsequent use;
(2) high temperature melting: being dropped in smelting furnace by the silicon ore containing impurity, is melt under the environment of 1700 DEG C ~ 1800 DEG C in temperature;
(3) oxygen blast refining: keep the temperature in smelting furnace to remain on 1600 DEG C ~ 1700 DEG C, the oxygen of abundance is passed in silicon water;
(4) sampling detects: keep the temperature in smelting furnace to remain on 1600 DEG C ~ 1650 DEG C, waits when being refined to a certain degree, sampling analysis aluminium content;
(5) degree of depth is except aluminium: detect through sampling, in silicon water, aluminium content is between 20% ~ 30%, and the wad a quilt with cotton ratio of agent of the combination in described silicon water and step (1) is Gui Shui ﹕ Lvization Mei ﹕ sodium carbonate=2500 ﹕ 21 ﹕ 30; Open fire door and release silicon water, when silicon water flows to silicon bag three/start to drop into 1/3rd of ready combination dealumination agent total amount for the moment, silicon water drops into 1/3rd of ready combination dealumination agent total amount again when flowing to silicon bag 2/3rds, silicon water drops into 1/3rd of ready combination dealumination agent total amount again when flowing to silicon bag 4/5ths, keep silicon water temp at about 1650 DEG C in the process that feeds intake, and need to complete in 30 minutes.
(6) filtering and impurity removing: by the degree of depth except the slag removing in the silicon water after aluminium, in the silicon water of gained, aluminium content is 0.17%.
Example 3
Carry out according to following steps:
(1) combination wadding agent configuration: magnesium chloride and sodium carbonate are mixed into according to a certain percentage the agent of combination wadding for subsequent use;
(2) high temperature melting: being dropped in smelting furnace by the silicon ore containing impurity, is melt under the environment of 1700 DEG C ~ 1800 DEG C in temperature;
(3) oxygen blast refining: keep the temperature in smelting furnace to remain on 1600 DEG C ~ 1700 DEG C, the oxygen of abundance is passed in silicon water;
(4) sampling detects: keep the temperature in smelting furnace to remain on 1600 DEG C ~ 1650 DEG C, waits when being refined to a certain degree, sampling analysis aluminium content;
(5) degree of depth is except aluminium: detect through sampling, in silicon water, aluminium content is more than 30%, and the wad a quilt with cotton ratio of agent of the combination in described silicon water and step (1) is Gui Shui ﹕ Lvization Mei ﹕ sodium carbonate=2500 ﹕ 40 ﹕ 57; Open fire door and release silicon water, when silicon water flows to silicon bag three/start to drop into 1/3rd of ready combination dealumination agent total amount for the moment, silicon water drops into 1/3rd of ready combination dealumination agent total amount again when flowing to silicon bag 2/3rds, silicon water drops into 1/3rd of ready combination dealumination agent total amount again when flowing to silicon bag 4/5ths, keep silicon water temp at about 1650 DEG C in the process that feeds intake, and need to complete in 30 minutes;
(6) filtering and impurity removing: by the degree of depth except the slag removing in the silicon water after aluminium, in the silicon water of gained, aluminium content is 0.18%.
Claims (3)
1. a method for metallic silicon smelting deep impurity-removing, is characterized in that, carries out according to following steps:
(1) combination wadding agent configuration: magnesium salts and sodium salt are mixed into according to a certain percentage the agent of combination wadding for subsequent use;
(2) high temperature melting: being dropped in smelting furnace by the silicon ore containing impurity, is melt under the environment of 1700 DEG C ~ 1800 DEG C in temperature;
(3) oxygen blast refining: keep the temperature in smelting furnace to remain on 1600 DEG C ~ 1700 DEG C, the oxygen of abundance is passed in silicon water;
(4) sampling detects: keep the temperature in smelting furnace to remain on 1600 DEG C ~ 1650 DEG C, waits when being refined to a certain degree, sampling analysis aluminium content;
(5) degree of depth is except aluminium: if in silicon water during aluminium content >=11%, open fire door and release silicon water, when silicon water flows to silicon bag three/start to drop into 1/3rd of ready combination dealumination agent total amount for the moment, silicon water drops into 1/3rd of ready combination dealumination agent total amount again when flowing to silicon bag 2/3rds, silicon water drops into 1/3rd of ready combination dealumination agent total amount again when flowing to silicon bag 4/5ths, keep silicon water temp at about 1650 DEG C in the process that feeds intake, and need to complete in 30 minutes;
(6) filtering and impurity removing: by the degree of depth except the slag removing in the silicon water after aluminium.
2. according to the method for a kind of metallic silicon smelting deep impurity-removing described in claim 1, it is characterized in that, in the agent of described step (1) combination wadding, the outfit ratio of magnesium salts and sodium salt is carried out as follows:
(1) when aluminium content is between 11% ~ 19%, Gui Shui ﹕ Mei Yan ﹕ sodium salt=2500 ﹕ 14 ﹕ 30;
(2) when aluminium content is between 20 ~ 30%, Gui Shui ﹕ Mei Yan ﹕ sodium salt=2500 ﹕ 21 ﹕ 30;
(3) when aluminium content is more than 30%, Gui Shui ﹕ Mei Yan ﹕ sodium salt=2500 ﹕ 40 ﹕ 57.
3. according to the method for a kind of metallic silicon smelting deep impurity-removing described in claim 1, it is characterized in that, described magnesium salts is magnesium chloride, and sodium salt is sodium carbonate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108946737A (en) * | 2018-07-23 | 2018-12-07 | 云南省龙陵县龙山硅有限责任公司 | A kind of method of metallic silicon smelting deep impurity-removing |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1143605A (en) * | 1995-08-22 | 1997-02-26 | 李忠莆 | Producing technique for refined silicon |
| CN101671027A (en) * | 2009-09-29 | 2010-03-17 | 包头市山晟新能源有限责任公司 | Metallurgical silicon purification method and on-line slagging boron removal method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1143605A (en) * | 1995-08-22 | 1997-02-26 | 李忠莆 | Producing technique for refined silicon |
| CN101671027A (en) * | 2009-09-29 | 2010-03-17 | 包头市山晟新能源有限责任公司 | Metallurgical silicon purification method and on-line slagging boron removal method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108946737A (en) * | 2018-07-23 | 2018-12-07 | 云南省龙陵县龙山硅有限责任公司 | A kind of method of metallic silicon smelting deep impurity-removing |
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Inventor after: Lin Zude Inventor after: Ding Weimin Inventor after: Zhou Jihong Inventor before: Zhou Jihong Inventor before: Ding Weimin Inventor before: Lin Zude |
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