KR102237891B1 - Method for manufacturing silicone additives, deoxidizer and desulfurizer by using silicone powder - Google Patents

Abstract

The provisional regulation, deoxidation, and desulfurization production method using silicon powder according to the present invention comprises the steps of preparing a raw material containing silicon powder recovered from industrial by-products or waste sludge, and manganese ( Mixing Mn), performing a milling process to produce a mixture in which the raw material and the manganese are uniformly mixed, mixing a binder for homogeneous binding between the raw material and the manganese, and the bonding Comprising the steps of compressing the blended mixture at high pressure to form briquettes and pellets, drying the briquettes and pelletized mixtures under a predetermined temperature condition, and applying an antioxidant to the dried monoliths. can do.

Description

Temporary regulation, deoxidation and desulfurization manufacturing method using silicon powder {METHOD FOR MANUFACTURING SILICONE ADDITIVES, DEOXIDIZER AND DESULFURIZER BY USING SILICONE POWDER}

The present invention relates to a method of manufacturing a temporary regulation, deoxidation and desulfurization agent used in a steel making process, and more particularly, when cutting an ingot for manufacturing (production) of a solar wafer or a semiconductor wafer. It relates to a method for preparing a temporary regulation, deoxidation and desulfurization agent using silicon powder capable of producing a temporary regulation, deoxidation and desulfurization agent using silicon sludge, which is a by-product generated (discharged).

As is well known, wafers in the solar cell or semiconductor industry are manufactured by cutting (cutting) a silicon ingot using, for example, a diamond saw with cutting oil. Sludge is generated.

In recent years, considering the situation in which the solar wafer silicon industry is rapidly growing as a new energy industry, it is expected that the amount of such silicon sludge will be further increased.

The silicon recovered from such sludge has a silicon content of 70 to 97%, and can be used as a deoxidizer and a silicon source, an energy source of a blast furnace, a converter, etc., and in cast iron and castings, silicon can be used as an additive to increase the silicon component.

That is, process sludge is a subsidiary material that not only has a relatively higher silicon content than conventional SiC-containing sludge, but also has excellent reaction power as a silicon source of molten steel, a deoxidizer, and a deoiling agent.

Although there have been attempts to produce and use such silicon as briquettes, there are cases where it is ignited during production or a fire occurs during transport or storage, so the usability review has not been actively conducted, but the silicon content is approximately 70 to 97%. Considering that it is relatively excellent so far and the solar energy industry continues to develop, it is absolutely required to use briquettes and pellets as conventional landfill treatment is not a waste of resources, but a large loss.

In relation to this, many studies have been conducted on the separation and recovery method of useful components until now, and in particular, there have been a number of studies on the recovery of silicon carbide (SiC) generated from the wire saw and its briquetting. In the activation of 1500 to 2400° C., the briquette product of silicon carbide had a limit of practicality because its use effect was extremely limited due to the melting point of high temperature.

Korean Patent Registration No. 10-1292001 (announcement date: 2013. 08. 05.)

An object of the present invention is to provide a method of manufacturing a temporary regulation, deoxidation, and desulfurization agent using silicon powder capable of improving reactivity with molten steel during a provision process using silicon sludge generated when a silicon wafer is produced using diamond saw.

An object of the present invention is to provide a method of manufacturing a temporary regulation, deoxidation, and desulfurization agent using silicon powder that can improve transport, transport, and usability using silicon sludge generated when a silicon wafer is produced using diamond saw.

The problem to be solved by the present invention is not limited to those mentioned above, and another problem to be solved that is not mentioned can be clearly understood by those of ordinary skill in the art from the following descriptions. will be.

The present invention, according to one aspect, preparing a raw material containing silicon powder recovered from industrial by-products or waste sludge, mixing manganese (Mn) for the specific gravity control and desulfurization effect of the prepared raw material, and milling Proceeding through a process to produce a mixture in which the raw material and the manganese are uniformly mixed, mixing a binder for homogeneous bonding between the raw material and the manganese, and compressing the mixture in which the binder is mixed at high pressure. Temporary regulation and deoxidation using silicon powder comprising the steps of briquetting and pelletizing, drying the briquetting and pelletized mixture under a predetermined temperature condition, and applying an antioxidant to the dried briquette And it can provide a method for producing a desulfurization agent.

The raw material of the present invention is a silicon source comprising at least one of silicon metal powder, silicon metal slag powder, waste furnace silicon powder, and silicon carbide powder This may be a mixed mixture.

The silicon source of the present invention may be blended in the range of 5 to 30 wt%.

The silicon source of the present invention may function as an oxidation stabilizer for minimizing the oxidation reaction of the silicon powder.

The manganese of the present invention may include one or more of manganese powder, silicon manganese powder, and depleted manganese (FeMn).

The manganese of the present invention may function to suppress the brittleness and bubble generation of steel that may occur during the steelmaking process.

The binder of the present invention may be an inorganic binder.

The inorganic binder of the present invention may be mixed in the range of 1 to 5wt%.

The inorganic binder of the present invention may contain one or more of bentonite, dextrin, and corn starch.

The drying step of the present invention may be performed under process conditions in a temperature range of 80 to 120°C and a time range of 1 to 2H.

The drying step of the present invention may be dried so that the breaking strength of the briquette and pelletization is 20Mpa or more.

The antioxidant of the present invention may be applied in a thickness range of 0.05 to 0.1mm.

According to an embodiment of the present invention, by manufacturing a temporary regulation, deoxidation and desulfurization agent that can improve the reactivity with molten steel during the provision process using silicon sludge generated when producing a silicon wafer using diamond saw, the cost of a steel member It is possible to reduce the cost, and it is possible to effectively reduce the treatment cost of silicon sludge for landfill.

1 is a flow chart showing a main process of manufacturing a temporary regulation, deoxidation and desulfurization agent using silicon powder recovered from industrial by-products or waste sludge according to an embodiment of the present invention.

First, the advantages and features of the present invention, and a method of achieving them will become apparent with reference to embodiments to be described later in detail together with the accompanying drawings. Here, the present invention is not limited to the embodiments disclosed below, but may be implemented in a variety of different forms, and only these embodiments are intended to complete the disclosure of the present invention, and are common in the technical field to which the present invention pertains. It is provided by way of example in order for those skilled in the art to clearly understand the scope of the invention, so the technical scope of the invention should be defined by the claims.

In addition, in the following description of the present invention, if it is determined that a detailed description of known functions or configurations may unnecessarily obscure the subject matter of the present invention, a detailed description thereof will be omitted. In addition, terms to be described later are terms defined in consideration of functions in the present invention, which may vary according to the intention or custom of users or operators. Therefore, the definition should be made based on the technical idea described throughout the present specification.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.

1 is a flow chart showing a main process of manufacturing a temporary regulation, deoxidation and desulfurization agent using silicon powder recovered from industrial by-products or waste sludge according to an embodiment of the present invention.

Raw material preparation step (step 102)

In step 102, raw materials containing silicon powder recovered from industrial by-products or waste sludge are prepared, for example, silicon sludge, which is a by-product discharged when producing silicon wafers for solar cells or semiconductors, is collected and prepared as a raw material. Here, silicon sludge (raw material) contains a large amount of silicon (Si) and moisture.

And, such a raw material is, for example, silicon metal powder (Si Metal powder), silicon metal slag powder (Si Metal slag powder), a silicon source containing one or more of the closed silicon powder (FeSi powder), silicon carbide powder (SiC powder) This may be a mixed mixture.

Here, the silicon source is preferably blended into the raw material in the range of, for example, 5 to 30 wt%, and this silicon source can function as an oxidation stabilizer for minimizing the oxidation reaction of the silicon powder.

In other words, silicon sludge generated in the silicon wafer cutting process during the production of conventional solar wafers is generated by using SiC wire saws, and contains relatively stable SiC, but recently diamond saws are used. Depending on the silicon powder (powder) of 70 to 95% comes out from the silicon sludge, and the silicon powder that comes out when polishing the cut wafer is also 85 to 95 wt% of high purity silicon, and the average particle size of the recovered silicon at this time It is about 20㎛.

However, due to the high purity and high possibility of oxidation upon contact with air or moisture and fine particle size, there may be a problem in that the bonding strength is deteriorated in case of briquette and pelletization.

In order to solve this problem, in the present invention, silicon metal stabilized in air and moisture containing silicon, slag thereof, by-products, ferrosilicon or its slag, by-products, silicon carbide, and the like are used as a source of Si.

Manganese (Mn) blending step (104)

In step 104, a valuable metal for specific gravity control and desulfurization effect, that is, manganese (Mn) may be mixed with the collected raw material (raw material containing silicon powder), such manganese is, for example, manganese powder, silicon It may contain one or more of manganese powder (SiMn powder) and decomposed manganese (FeMn), and from a functional aspect, the blended manganese will function to suppress the brittleness and bubble generation of steel that may occur during the steelmaking process. I can.

That is, silicon powder, for example, has a specific gravity of 0.8 to 1.1 mg/ml, so it may float when added to the molten steel, so that the reaction occurs only in the upper part of the molten metal, and the reaction in the deep part may not be smooth. Additionally blended raw material with high specific gravity (manganese)

In particular, manganese powder (eg, manganese powder, silicon manganese powder, closed manganese, etc.) may be added to supplement the specific gravity and manganese, which plays a large role in the steelmaking process.

Here, in the case of manganese, it can play an exclusive role as the highest silicon recovery rate and desulfurization agent, and can play a role (function) of increasing the yield of the steel making process and reducing the amount of solvent consumption.

In addition, manganese can play a specific gravity and chemical role by preventing corrosion of furnace refractories and extending the lifespan, and can play a role of improving the quality of steel products by preventing brittleness and air bubbles in the final steel product. .

In addition, since the average particle size of the recovered silicon is fine, for example, 20 μm, and the bonding strength between the particles is weak, it is preferable to mix manganese by adjusting the particle size to 0 to 5 mm.

Milling step 106 for homogeneous mixing

In step 106, a milling process is performed to produce a mixture in which the raw material (raw material containing silicon powder) and manganese are uniformly mixed, for example, so that the difficulty of mixing due to the difference in specific gravity can be solved, for example, a vertical interlocking mixer, a screw. After mixing using an anticorrosive mixer, a double spatula mixer, etc., a milling process is performed to produce a homogeneous mixture.

Binder (or adhesive) mixing step 108

In step 108, a binder (or adhesive) for homogeneous bonding between the raw material (silicone powder-containing raw material) and manganese is mixed (added), wherein the binder is, for example, an inorganic binder in the range of 1 to 5 wt%. The inorganic binder may include, for example, one or more of bentonite, dextrin, and corn starch.

That is, the recovered silicon and the material blended therein are not uniformly mixed when mixing by adding an inorganic binder (binder) with a difference in specific gravity of 5 or more, so for uniform mixing, the embodiment of the present invention In, for example, a propeller type mixer that can rotate 360 degrees has a function that allows it to move up and down, so that it can be uniformly mixed regardless of the specific gravity.

Here, uniform mixing is an important factor in the quality of briquettes and pellets, so it can be said to be a very important production process.

And, as a binder (adhesive), for example, bentonite, dextrin, corn starch, etc. can be used, but when added to a converter or LF (Ladle Furnace), the smog phenomenon should be reduced as much as possible to improve workability. It can reduce the occurrence.

At this time, in order to reduce oxidation that may occur in subsequent processes (eg, briquetting and pelletizing processes), an antioxidant may be mixed with a binder.

Briquetting and pelletizing step (110)

In step 110, the mixture in which the binder (or adhesive) is mixed is compressed to form briquettes and pellets, and the briquetting and pelletizing process is for increasing strength and rapid reaction in the molten metal. Here, briquetting and pelletizing may be performed by a hydraulic press method.

That is, since the average particle size of the recovered silicon, which is the main component of the raw material, is fine at 20 µm, it can float when added directly to the molten metal, so it is molded and used. At this time, even if a binder (adhesive) is used, the bonding strength between particles, briquettes, and In order to increase the strength, the briquetting and pelletizing process can be carried out using hydraulic press briquetting equipment or extrusion pelleting equipment.

In this case, when the length of the briquette is 20 to 40 mm and the diameter is 25 mm or less, drying can be performed well without loss of silicon during drying in a subsequent drying process.

In addition, the length of the pellet is about 5 to 30 mm and the diameter is about 8 mm, so that it can be dried well without loss of silicon, as well as to be used in a process in which the reaction must be terminated in, for example, 15 to 30 minutes.

As such, in the case of pellets, since the surface area is large, it is possible to induce a reaction in the molten steel so that it does not float in the molten steel and diffuses quickly, and through such rapid diffusion, the yield of a deoxidizer, a desulfurization agent and silicon can be maximized.

Drying step (112)

In step 112, the briquette and pelletized mixture is dried (press-molded) under a predetermined temperature condition, and this drying process may be performed, for example, in a temperature range of 80 to 120°C and a process condition in the range of 1 to 2H time. have.

Here, the breaking strength of briquettes and pellets obtained through the drying process may be, for example, 20 Mpa or more.

That is, since silicon has a relatively high affinity with air and moisture, it is easily oxidized or may be ignited due to heat generated by this oxidation reaction, and thus a drying process is performed to prevent this.

In addition, when the drying process temperature is 120°C or higher, the affinity between air and moisture increases rapidly. Therefore, the drying process temperature is preferably 80 to 120°C, for example.

Antioxidant application step (114)

In step 114, an antioxidant may be applied to the dried briquette to prevent oxidation of silicon (for oxidation stability of silicon), wherein the applied antioxidant is, for example, in a thickness range of 0.05 to 0.1 mm. I can have it.

Here, the temporary regulation, deoxidation and desulfurization agent coated with an antioxidant of a predetermined thickness may be dried at room temperature.

The above description is merely illustrative of the technical idea of the present invention, and those of ordinary skill in the technical field to which the present invention pertains, various substitutions, modifications and changes, etc., within the scope not departing from the essential characteristics of the present invention. It will be easy to see that this is possible. That is, the embodiments disclosed in the present invention are not intended to limit the technical idea of the present invention, but to explain the technical idea, and the scope of the technical idea of the present invention is not limited by these embodiments.

Accordingly, the scope of protection of the present invention should be interpreted by the claims to be described later, and all technical thoughts within the scope equivalent thereto should be construed as being included in the scope of the present invention.

Claims (12)

Preparing a raw material containing silicon powder recovered from industrial by-products or waste sludge, and
Blending manganese (Mn) for controlling the specific gravity of the prepared raw material, preventing floating of the recovered silicon powder, and desulfurizing effect, and
Producing a mixture in which the raw material and the manganese are uniformly mixed by performing a milling process, and
Mixing a binder for homogeneous bonding between the raw material and the manganese,
Compressing the mixture in which the binder is mixed at high pressure to make briquettes and pellets,
Drying the briquette and pelletized mixture under a predetermined temperature condition,
Including the step of applying an antioxidant to the dried briquette,
The manganese includes silicon manganese powder (SiMn powder),
Temporary regulation, deoxidation and desulfurization manufacturing method using silicon powder. The method of claim 1,
The raw material is,
Silicon metal powder (Si Metal powder), silicon metal slag powder (Si Metal slag powder), closed furnace silicon powder (FeSi powder), silicon carbide powder (SiC powder) is a mixture of a silicon source containing at least one of the mixture
Temporary regulation, deoxidation and desulfurization manufacturing method using silicon powder. The method of claim 2,
The silicon source,
Blended in the range of 5 to 30 wt%
Temporary regulation, deoxidation and desulfurization manufacturing method using silicon powder. The method of claim 2,
The silicon source,
Functioning as an oxidation stabilizer to minimize the oxidation reaction of the silicon powder
Temporary regulation, deoxidation and desulfurization manufacturing method using silicon powder. The method of claim 1,
The manganese is,
Further comprising at least one of manganese powder (Mn powder) and decomposed manganese (FeMn),
Temporary regulation, deoxidation and desulfurization manufacturing method using silicon powder. The method of claim 5,
The manganese is,
It functions to suppress the brittleness and bubble generation of steel that may occur during the steelmaking process.
Temporary regulation, deoxidation and desulfurization manufacturing method using silicon powder. The method of claim 1,
The binder,
Inorganic Binder In
Temporary regulation, deoxidation and desulfurization manufacturing method using silicon powder. The method of claim 7,
The inorganic binder,
Blended in the range of 1 to 5 wt%
Temporary regulation, deoxidation and desulfurization manufacturing method using silicon powder. The method of claim 7,
The inorganic binder,
Containing one or more of bentonite, dextrin, corn starch
Temporary regulation, deoxidation and desulfurization manufacturing method using silicon powder. The method of claim 1,
The drying step,
80 to 120 ℃ temperature range and 1 to 2H performed in the process conditions of the time range
Temporary regulation, deoxidation and desulfurization manufacturing method using silicon powder. The method of claim 1,
The drying step,
Drying so that the breaking strength of the briquette and pelletization is 20Mpa or more
Temporary regulation, deoxidation and desulfurization manufacturing method using silicon powder. The method of claim 1,
The antioxidant,
Applied in a thickness range of 0.05 to 0.1 mm
Temporary regulation, deoxidation and desulfurization manufacturing method using silicon powder.

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