CN111591996B - Method for preparing industrial silicon by using ferrosilicon - Google Patents
Method for preparing industrial silicon by using ferrosilicon Download PDFInfo
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- CN111591996B CN111591996B CN202010669692.4A CN202010669692A CN111591996B CN 111591996 B CN111591996 B CN 111591996B CN 202010669692 A CN202010669692 A CN 202010669692A CN 111591996 B CN111591996 B CN 111591996B
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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
- C01B33/021—Preparation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/16—Controlling or regulating processes or operations
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C3/00—Removing material from alloys to produce alloys of different constitution separation of the constituents of alloys
- C22C3/005—Separation of the constituents of alloys
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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
Abstract
The invention relates to a method for preparing industrial silicon by using a ferrosilicon alloy, belonging to the technical field of industrial silicon smelting. The method comprises the steps of continuously adding a ferrosilicon melt into a directional solidification fixed casting device at a constant speed, controlling the temperature, flow rate and solidification speed of the ferrosilicon melt to realize segregation and enrichment of metallic iron, obtaining silicon ingot products with iron content in step distribution, sampling and detecting the silicon ingot products, determining nodes with Fe content in step distribution, and carrying out grading treatment on the silicon ingot to obtain various levels of industrial silicon products with different iron mass contents, wherein the industrial silicon products comprise chemical-level industrial silicon, metallurgical-level industrial silicon and ferrosilicon. The method directly removes iron from the ferrosilicon melt with high efficiency, can purify the ferrosilicon part to industrial silicon, and has the characteristics of low production cost, wide technical adaptability, wide application prospect and the like.
Description
Technical Field
The invention relates to a method for preparing industrial silicon by using a ferrosilicon alloy, belonging to the technical field of industrial silicon smelting.
Background
In the existing silicon industry, ferrosilicon faces the situation of excess productivity. In addition, the price of the ferrosilicon is basically kept to be 5500-6200 yuan/ton, while the price of the industrial silicon, the quality of the normal grade product, such as the price of 441# industrial silicon, is basically stabilized to be more than 10000 yuan/ton. If the ferrosilicon is used as the raw material and the corresponding silicon separation technology is used as the auxiliary material, not only the ferrosilicon and industrial silicon products can be obtained simultaneously, but also the profit margin of the industrial silicon products can be stably promoted, and value-added service is provided for the ferrosilicon industry.
In the existing industrial silicon purification technology, the separation of metal impurities such as iron in silicon is realized by a controllable solidification mode based on a directional solidification technology of a segregation theory; the aim of enriching the impurity Fe into a post-solidification liquid phase is realized through a controllable solidification process, and then the silicon of a pre-solidification part obtains higher purity. However, in the aspect of the casting process of the melt in the industrial silicon industry, the natural air cooling type solidification technology is always adopted, the silicon-iron alloy melt refined by ladle oxygen blowing is directly poured into an ingot mould, and a silicon ingot product is formed through natural cooling. The solidification mode is greatly influenced by factors such as ingot mold structure, melt component fluctuation, manual operation in the casting process and the like, so that different degrees of component segregation are generated in the silicon-iron alloy melt die casting process, the uniformity of industrial silicon products is obviously influenced, and the product quality grade determined according to random sampling detection results and the real product quality are greatly different; therefore, the existing intermittent solidification forming technology cannot meet the continuous controllable requirement of the directional solidification Fe removing technology.
The existing polysilicon ingot casting technology cannot be directly applied to the industrial silicon production process because the equipment cost and the equipment running cost of polysilicon ingot casting are high, the intermittent production period is long, and the existing polysilicon ingot casting technology cannot be effectively grafted with the industrial silicon industry with low-cost space and a continuous production mode.
Disclosure of Invention
The invention provides a method for preparing industrial silicon by using a silicon iron alloy, aiming at the problem of insufficient profit space of products obtained by the existing industrial silicon production process, the method fully utilizes the cost advantage of the production of silicon iron products, realizes the segregation and separation of iron elements with segregation coefficient far less than 1 in main silicon by introducing the silicon iron as a direct raw material for the production of the industrial silicon and controlling the casting and solidification processes of silicon iron melt, and can bring huge economic benefit by controlling the process cost when the product with the brand number of FeSi90Al3.0 of the silicon iron is converted into two products of Si441 and FeSi75Al0.5-A.
The invention can convert the low-price ferrosilicon into industrial silicon products, can reduce the cost of the existing industrial silicon production and smelting process, improve the ingot casting efficiency and the product quality, and greatly reduce the dependence of the industrial silicon product quality on raw materials.
A method for preparing industrial silicon by using ferrosilicon comprises the following specific steps:
the method comprises the steps of continuously adding a ferrosilicon alloy melt into a directional solidification fixed casting device at a constant speed, controlling the temperature, the flow rate and the solidification speed of the ferrosilicon alloy melt to realize segregation and enrichment of metallic iron, obtaining silicon ingot products with iron content in step distribution, carrying out sampling detection on the silicon ingot products, determining nodes with the Fe content in step distribution, carrying out grading treatment on the silicon ingots to obtain various levels of industrial silicon products with different iron mass contents, and removing unqualified intermediate products to obtain the silicon ingot products comprising chemical-level industrial silicon, metallurgical-level industrial silicon and ferrosilicon.
The ferrosilicon alloy melt is 90# ferrosilicon alloy and/or ferrosilicon alloy of more than 90# trade mark.
The temperature of the ferrosilicon alloy melt is 1450-1750 ℃, the flow rate of the ferrosilicon alloy melt is 0.1-10 kg/s, and the directional solidification speed is 0.1-5 cm/s.
Based on the total mass of the finally obtained silicon ingot product as 100%, the chemical-grade industrial silicon product is not less than 40%, the metallurgical-grade industrial silicon product is not less than 50%, and the ferrosilicon alloy product is not more than 10%.
The invention has the beneficial effects that:
(1) The invention adopts the ferrosilicon melt obtained by electric furnace production as the raw material to replace the prior process of preparing the industrial silicon melt by the carbothermic reduction of a high-purity silica raw material and a carbonaceous reducing agent submerged arc electric furnace, and simultaneously controls the segregation deposition of impurity elements in the ferrosilicon melt aiming at the controllable continuous melt cooling rate and the controllable ingot casting rate of the ferrosilicon melt obtained by furnace discharge, so that the ferrosilicon melt is enriched into the uncrystallized tail melt by strengthening segregation, thereby reducing the impurity content in the high-silicon product which is solidified firstly;
(2) The method solves the problems that the high-quality industrial silicon product is controlled by the purity of the raw materials, the industrial silicon and the ferrosilicon have small profit margin in smelting, and the like, and simultaneously realizes the purpose of increasing the value of the high-quality industrial silicon product prepared from the cheap ferrosilicon raw material.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: as shown in figure 1, the method for preparing the industrial silicon by using the ferrosilicon alloy comprises the following specific steps:
(1) Continuously and uniformly adding a FeSi90Al3.0-A # ferrosilicon melt obtained by smelting in a submerged arc electric furnace into a solidification and fixed casting device, adjusting the supercooling degree and the directional solidification speed of the directional solidification and continuous casting device according to the size and the real-time temperature of the melt of the directional solidification and continuous casting device, continuously feeding and continuously discharging ingots, and promoting the Fe impurity with the segregation coefficient far smaller than 1 in the ferrosilicon melt to be continuously segregated into the uncrystallized melt of the directional solidification and continuous casting device to obtain a silicon ingot product with iron content in step distribution; wherein the temperature of the ferrosilicon alloy melt to be deironized is 1750 ℃, the flow rate of the ferrosilicon alloy melt is 0.1kg/s, and the directional solidification speed is 0.1cm/s;
(2) Sampling and detecting the silicon ingot products obtained in the step (1), determining the nodes with the gradient distribution of the Fe content, carrying out grading treatment on the silicon ingot to obtain all-grade industrial silicon products with different iron quality contents and intermediate products which do not accord with quality grade identification, and returning the intermediate products which do not accord with the quality grade identification to smelting and then carrying out continuous ingot casting treatment; the industrial silicon products comprise chemical-grade industrial silicon, metallurgical-grade industrial silicon and ferrosilicon;
the quality of the ferrosilicon alloy melt produced by the submerged arc electric furnace in the embodiment before and after Fe removal is shown in Table 1,
TABLE 1 comparison of results before and after continuous ingot casting of a ferrosilicon melt, wt. -%)
Based on 100 percent of the total mass of the silicon ingot product obtained after the unqualified intermediate product is removed, the chemical-grade industrial silicon accounts for 44 percent, the metallurgical-grade industrial silicon accounts for 53 percent, and the silicon iron alloy FeSi accounts for 3 percent.
Example 2: as shown in fig. 1, a method for preparing industrial silicon by using a silicon-iron alloy comprises the following specific steps:
(1) Continuously and uniformly adding a FeSi90Al3.0-A # ferrosilicon melt obtained by smelting in a submerged arc electric furnace into a solidification and fixed casting device, adjusting the supercooling degree and the directional solidification speed of the directional solidification and continuous casting device according to the size and the real-time temperature of the melt of the directional solidification and continuous casting device, continuously feeding and continuously discharging ingots, and promoting the Fe impurity with the segregation coefficient far smaller than 1 in the ferrosilicon melt to be continuously segregated into the uncrystallized melt of the directional solidification and continuous casting device to obtain a silicon ingot product with iron content in step distribution; wherein the temperature of the ferrosilicon alloy melt to be deironized is 1600 ℃, the flow rate of the ferrosilicon alloy melt is 5kg/s, and the directional solidification speed is 2.5cm/s;
(2) Sampling and detecting the silicon ingot products obtained in the step (1), determining the nodes with the gradient distribution of the Fe content, carrying out grading treatment on the silicon ingot to obtain all-grade industrial silicon products with different iron quality contents and intermediate products which do not accord with quality grade identification, and returning the intermediate products which do not accord with the quality grade identification to smelting and then carrying out continuous ingot casting treatment; the industrial silicon products comprise chemical-grade industrial silicon, metallurgical-grade industrial silicon and ferrosilicon;
the quality of the ferrosilicon alloy melt produced by the submerged arc electric furnace in the embodiment before and after Fe removal is shown in Table 2,
TABLE 2 comparison of results before and after continuous ingot casting of the ferrosilicon melt, wt. -%)
Based on 100% of the total mass of the silicon ingot product obtained after the unqualified intermediate product is removed, the chemical-grade industrial silicon accounts for 35%, the metallurgical-grade industrial silicon accounts for 41%, the ferrosilicon alloy FeSi accounts for 52%, and the intermediate product which does not meet the quality grade identification accounts for 7%.
Example 3: as shown in fig. 1, a method for preparing industrial silicon by using a silicon-iron alloy comprises the following specific steps:
(1) Continuously and uniformly adding a FeSi90Al3.0-A # ferrosilicon melt obtained by smelting in a submerged arc electric furnace into a solidification and fixed casting device, adjusting the supercooling degree and the directional solidification speed of the directional solidification and continuous casting device according to the size and the real-time temperature of the melt of the directional solidification and continuous casting device, continuously feeding and continuously discharging ingots, and promoting the Fe impurity with the segregation coefficient far smaller than 1 in the ferrosilicon melt to be continuously segregated into the uncrystallized melt of the directional solidification and continuous casting device to obtain a silicon ingot product with iron content in step distribution; wherein the temperature of the ferrosilicon alloy melt to be deironized is 1450 ℃, the flow rate of the ferrosilicon alloy melt is 10kg/s, and the directional solidification speed is 5cm/s;
(2) Sampling and detecting the silicon ingot products obtained in the step (1), determining the nodes with the gradient distribution of the Fe content, carrying out grading treatment on the silicon ingot to obtain all-grade industrial silicon products with different iron quality contents and intermediate products which do not accord with quality grade identification, and returning the intermediate products which do not accord with the quality grade identification to smelting and then carrying out continuous ingot casting treatment; the industrial silicon products comprise chemical-grade industrial silicon, metallurgical-grade industrial silicon and ferrosilicon;
the quality of the ferrosilicon melt produced by the submerged arc electric furnace in this example before and after the removal of Fe is shown in Table 3,
TABLE 3 comparison of results before and after continuous ingot casting of the ferrosilicon melt, wt. -%)
By taking the total mass of the silicon ingot product obtained after the unqualified intermediate product is removed as 100%, the chemical-grade industrial silicon accounts for 40%, the metallurgical-grade industrial silicon accounts for 50%, the silicon iron alloy FeSi accounts for 20%, and the intermediate product which does not meet the quality grade identification accounts for 10%.
Claims (4)
1. A method for preparing industrial silicon by using ferrosilicon is characterized by comprising the following specific steps:
the method comprises the steps of continuously adding a ferrosilicon melt into a directional solidification fixed casting device at a constant speed, controlling the temperature, flow rate and solidification speed of the ferrosilicon melt to realize segregation and enrichment of metallic iron, obtaining silicon ingot products with iron content in step distribution, carrying out sampling detection on the silicon ingot products, determining nodes with the Fe content in step distribution, and carrying out grading treatment on the silicon ingots to obtain various levels of industrial silicon products with different iron mass contents, wherein the industrial silicon products comprise chemical-level industrial silicon, metallurgical-level industrial silicon and ferrosilicon.
2. The method for preparing industrial silicon using ferrosilicon according to claim 1, wherein: the ferrosilicon alloy melt is No. 90 ferrosilicon alloy and/or ferrosilicon alloy with a grade above No. 90.
3. The method for preparing industrial silicon using ferrosilicon according to claim 1, wherein: the temperature of the ferrosilicon melt is 1450-1750 ℃, the flow rate of the ferrosilicon melt is 0.1-10 kg/s, and the directional solidification speed is 0.1-5 cm/s.
4. The method for preparing industrial silicon using ferrosilicon according to claim 1, wherein: based on the total mass of the industrial silicon product being 100%, the chemical grade industrial silicon product is not less than 40%, the metallurgical grade industrial silicon product is not less than 50%, and the ferrosilicon alloy product is not more than 10%.
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| CN101506097A (en) * | 2006-08-31 | 2009-08-12 | 三菱麻铁里亚尔株式会社 | Metallic silicon and process for producing the same |
| CN102040219A (en) * | 2009-10-14 | 2011-05-04 | 贵阳宝源阳光硅业有限公司 | Method for preparing high-purity silicon by purifying industrial silicon |
| CN102139879A (en) * | 2011-02-18 | 2011-08-03 | 厦门大学 | Method for purifying polysilicon by using silicon and tin alloy |
| CN102659110A (en) * | 2012-04-19 | 2012-09-12 | 厦门大学 | Method for directionally solidifying and purifying polycrystalline silicon by adopting ferro-silicon alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5104096A (en) * | 1988-02-17 | 1992-04-14 | Globe Metallurgical Inc. | Smelting apparatus for making elemental silicon and alloys thereof |
| FR2729131B1 (en) * | 1995-01-09 | 1997-02-14 | Pechiney Electrometallurgie | SILICON AND METALLURGIC FERROSILICON WITH LOW OXYGEN CONTENT |
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Patent Citations (6)
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|---|---|---|---|---|
| CN101506097A (en) * | 2006-08-31 | 2009-08-12 | 三菱麻铁里亚尔株式会社 | Metallic silicon and process for producing the same |
| CN102040219A (en) * | 2009-10-14 | 2011-05-04 | 贵阳宝源阳光硅业有限公司 | Method for preparing high-purity silicon by purifying industrial silicon |
| CN102139879A (en) * | 2011-02-18 | 2011-08-03 | 厦门大学 | Method for purifying polysilicon by using silicon and tin alloy |
| CN102659110A (en) * | 2012-04-19 | 2012-09-12 | 厦门大学 | Method for directionally solidifying and purifying polycrystalline silicon by adopting ferro-silicon alloy |
| CN105293502A (en) * | 2015-10-19 | 2016-02-03 | 成都理工大学 | Method for preparing solar-grade silicon by refining industrial silicon |
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