KR101890311B1 - Manufacturing method of heat increasing and component controlling briquette used in steel manufacturing process - Google Patents

Abstract

The present invention relates to a method for purifying waste slurries containing silicon to produce briquettes for controlling heat and composition for use in the process of manufacturing molten steel in a steelmaking process.
The present invention relates to an initial waste slurry containing silicon (Si), silicon carbide (SiC), water-soluble oil and iron (Fe) at a first mixing ratio, A first separation step of separating the water-soluble oil and the water from the waste slurry, and a binder in the Si-SiC-containing slurry obtained by separating the water-soluble oil and the water from the initial waste slurry through the primary separation step, And a briquetting step of forming a briquette after stirring. The volume median diameter (Dv 50) of the particles constituting the initial waste slurry is characterized by being 1 μm or more.
According to the present invention, it is possible to manufacture briquettes for heat treatment and component adjustment used in the process of manufacturing molten steel in the steelmaking process with low cost and high efficiency while minimizing environmental pollution.

Description

TECHNICAL FIELD [0001] The present invention relates to a briquetting method for briquette formation,

The present invention relates to a process for purifying and briquetting a waste slurry containing silicon (Si) and silicon carbide (SiC) to produce a briquette for regenerating and regulating components used in the steel making process of a steelmaking process ≪ / RTI > More particularly, the present invention relates to a process for purifying silicon waste slurry produced in the manufacture of semiconductor or solar cell wafers, thereby preventing generation of fire and effectively suppressing silicon oxidation in the process of manufacturing briquettes for controlling heat and components used in the steelmaking process To a briquetting regulating briquette used in a steelmaking process which enables a briquette-shaped briquetting process to be carried out easily, and a process for producing a heat-resisting and tempering regulator for steelmaking which is a raw material for the briquetting .

Generally, steelmaking process oxidizes impurities such as carbon in pig iron at a molten steel temperature of around 1500 degrees Celsius, and the oxide is removed by slag. In the steelmaking process, after a certain period of time from the start of oxygen blowing, the steel is exposed. At this time, manganese iron, silicon iron and the like are added for controlling and deoxidizing the components. At this time, a large amount of silicon is required to produce the added silicon iron, but the cost of the entire steelmaking process is increased because the price of silicon that is largely dependent on imports is high.

Generally, in order to increase the temperature in a furnace during a steelmaking process including a steelmaking process, silicon (Si) having excellent heat generation is used as a heat transfer agent. Due to the nature of the iron and steel industry, an enormous amount of silicon is required, but the price of silicon used as an exothermic agent is high.

On the other hand, as is well known, silicon is used as a main material of the semiconductor industry. When a semiconductor product is manufactured through various processes, a waste slurry containing a large amount of silicon is discharged as a by-product. When such a silicon-containing waste slurry is simply incinerated or buried in the soil, severe air pollution and soil contamination are caused. Therefore, a method of solidifying the silicon-containing waste slurry by cement and storing or embedding it is applied.

The discharge process of a waste slurry containing a large amount of silicon will be described in detail as follows.

Silicon wafers used in the manufacture of semiconductor integrated circuits and solar cells are produced by slicing the silicon ingot. In addition, the cut silicon wafer may be subjected to a surface polishing process to planarize the surface.

A slurry obtained by mixing silicon carbide (SiC), which is a cutting material, with coolant (water-soluble or oil-soluble cutting oil), is used for a cutting process of a silicon ingot, which is also called a wire sawing process. Silicon wafers can be produced by cutting a silicon ingot using a cutting tool called a wire saw in a state where the slurry is supplied. As the material of the cutting material, alumina (aluminum oxide), diamond, silicon dioxide, etc. may be used in addition to silicon carbide (silicon carbide).

Since the wire saw used in the cutting process of the silicon ingot has a certain thickness, a considerable amount of the silicon ingot is generated as a saw dust during the cutting process. As the thickness of the silicon wafer and the wire saw becomes thinner, Minute.

For example, if the thickness of the silicon wafer is 0.1 mm and the thickness of the wire saw is 0.1 mm, about 50% of the silicon ingot will be generated in the cut. Therefore, the waste slurry after the cutting process of the silicon ingot or the surface polishing process of the silicon wafer includes the abrasive differentiation such as cutting material, cutting oil, cutting powder, equipment and the like.

The silicon-containing waste slurry generated in the production of silicon wafers is classified as a special industrial waste. When the silicon-containing waste slurry is simply incinerated or buried, serious air pollution and soil contamination are caused. Therefore, And the method of storing or embedding is applied.

However, even if the method of solidifying with cement is used, there is a limitation in the storage space and the reclamation space, and there is a waste of resources. Therefore, a method for recycling and recycling the silicon-containing waste slurry is desperately required.

On the other hand, the silicon-containing waste slurry is composed of particles having various diameters. If the content of the fine particles is high, the following problems may occur in the course of recycling for the steelmaking process.

First, in the drying process for recycling the silicon-containing waste slurry, there is a problem in that there is a possibility of ignition due to the reaction between the silicon fine powder component and water.

Secondly, since the total surface area of silicon is increased and the contact area with oxygen is increased, the amount of silicon oxidation increases.

Thirdly, there is a problem that the strength of the briquette, which is a molded product in the form of a lump, is lowered, and the molded briquettes are easily broken.

Korean Patent Laid-Open Publication No. 10-2006-0028191 (Published Date: Mar. 29, 2006, titled: Recycling Apparatus and Method for Waste Sludge Generated in Semiconductor Wafer Manufacturing) Korean Patent Laid-Open Publication No. 10-2006-0059539 Disclosure Date: Jun. 02, 2006 Name: Regenerator for waste sludge generated during semiconductor wafer production) Korean Registered Patent No. 10-0776966 (registered name: November 09, 2007, titled: regeneration device for waste slurry generated in manufacturing semiconductor wafers)

The present invention relates to a method for producing a briquette for controlling the heat and composition used in a steelmaking process by purifying a waste slurry containing silicon generated in the production of semiconductor or solar cell wafers, And a method for manufacturing the same.

The present invention also relates to a method for manufacturing a briquetting briquetting apparatus for use in a steelmaking process capable of preventing the possibility of ignition due to the reaction of moisture with a silicon fine powder component which may occur during the reprocessing of a silicon- And a method for manufacturing a steelmaking heat and composition regulating material which is a raw material for the briquetting.

The present invention also relates to a method for producing briquettes for controlling heat and composition for use in a steelmaking process capable of effectively suppressing the amount of silicon oxidation in the course of reprocessing silicon-containing waste slurry, And to provide a method for manufacturing an adjustable body.

The present invention also relates to a method for manufacturing a briquetting heat controlling and regulating component for use in a steelmaking process capable of preventing a molded briquette from being broken due to a decrease in strength of a briquetting molded article, And to provide a method for manufacturing a steelmaking heat and component regulating body.

In addition, the present invention can recycle the silicon-containing waste slurry, which is an element of environmental pollution, as a briquetting heat for regenerating and controlling the components used in a steelmaking process without incineration or landfilling, thereby reducing waste disposal cost and cost competitiveness And to minimize the environmental pollution that may occur during the steelmaking process.

The present invention also relates to a method of manufacturing briquettes for controlling the heat and the components used in environmentally friendly steelmaking processes by extracting and reusing the water-soluble oil contained in the silicon waste slurry and purifying the discharged wastewater to a level that does not require reprocessing And a method for manufacturing a steelmaking heat and composition regulating material which is a raw material for the briquetting.

In addition, the present invention can optimize the amount of water to be mixed into the silicon waste slurry in the process of purifying the silicon waste slurry, thereby improving the efficiency of manufacturing the briquetting for regenerating and regulating the composition and reducing the reprocessing cost of the discharged wastewater It is another object of the present invention to provide a method for producing briquettes for controlling the heat and composition used in a steelmaking process and a method for manufacturing the briquetting heat and composition regulating material for steelmaking.

In addition, the present invention relates to a method for manufacturing a semiconductor wafer or a solar cell wafer, which comprises purifying a waste slurry containing silicon generated during the production of a semiconductor or a solar cell wafer to prepare a powder, adding a binder thereto and briquetting, And to provide a method for manufacturing a briquette for use and a steelmaking heat and composition regulating material which is a raw material of the briquette at low cost and high efficiency.

In addition, the present invention can reduce waste disposal cost by recycling the silicon waste slurry which is an element of environmental pollution, for incineration or landfilling, in the process of manufacturing molten steel in steel mills, And to secure cost competitiveness by cost reduction, while minimizing the environmental pollution that may occur during the steelmaking process.

In addition, the present invention reuses the wastewater containing water-soluble oil and water generated in the pulverization process of the silicon waste slurry as an additive necessary for manufacturing briquettes, thereby eliminating the need to reprocess the discharged wastewater, The method of making briquettes for heat treatment and composition control used in the process of manufacturing molten steel in the steelmaking process and the method of making environmentally friendly and economical production of the steelmaking heat and composition control material which is the raw material of the briquetting The technical problem is to provide.

In addition, the present invention provides a method for powdering a silicon waste slurry and molding the slurry into a briquettic material, thereby easily injecting it into the converter during the steelmaking process, and eliminating the risk of fire or explosion due to the powder.

The present invention relates to a method for producing a briquetting composition for regenerating heat and components used in the process of manufacturing molten steel by purifying a waste slurry containing silicon, A primary separation step of separating the water-soluble oil and the water from the initial waste slurry in a state where water is mixed with an initial waste slurry containing water-soluble oil and iron (Fe) at a preset first mixing ratio, And a briquetting step of adding a binder to the obtained Si-SiC-containing slurry obtained by separating the water-soluble oil and the water from the initial waste slurry, stirring the slurry, and molding the slurry into a briquette, The volume median diameter (Dv 50) of the particle group constituting the waste slurry is characterized by being 1 μm or more.

The first mixing ratio is set such that the volume of the water is 0.2 times or more and 8 times or less the volume of the initial waste slurry in the steelmaking process according to the present invention, .

The method for manufacturing a briquetting heat and composition for use in a steelmaking process according to the present invention is characterized in that water is added to the Si-SiC-containing slurry obtained through the primary separation step after the primary separation step and before the briquetting step 2 mixed ratio, and then filtering the water-soluble oil remaining in the Si-SiC-containing slurry.

The second mixing ratio is set so that the volume of the water is not less than 0.2 times and not more than 8 times the volume of the Si-SiC-containing slurry in the steelmaking process according to the present invention. .

The method for manufacturing a briquetting heat and composition for use in a steelmaking process according to the present invention is characterized in that after the first separation step, the water-soluble oil and water separated from the initial waste slurry are fractionally distilled through the first separation step, And a second separation step of separating the water and the water from each other.

The method for manufacturing a briquetting heat and composition for use in a steelmaking process according to the present invention further comprises a drying step of drying the Si-SiC-containing slurry obtained through the first separation step before the briquetting step do.

The briquetting method for controlling the heat and the composition used in the steelmaking process according to the present invention comprises grinding the Si-SiC-containing slurry dried through the drying step to obtain the Si-SiC-containing powder before the briquetting step And further comprising:

In the method for manufacturing a briquetting heat and composition for use in the steelmaking process according to the present invention, the diameter of the Si-SiC-containing powder obtained through the milling step is 5 cm or less.

In the method for manufacturing briquetting heat and composition for use in the steelmaking process according to the present invention, in the briquetting step, an iron source (Fe source) is further added to the Si-SiC containing slurry, , The Si-SiC-containing slurry is 30 wt% or more, and the iron component is 30 wt% or less.

In the first separation step, the initial waste slurry mixed and stirred with water is filtered by a pressing method to remove the water-soluble oil and the water-soluble oil from the initial waste slurry, And separating the water.

In the first separation step, centrifugation is applied to an initial waste slurry mixed with water to remove the water-soluble oil and water from the initial waste slurry, Is separated.

The present invention relates to a method for preparing a steelmaking heat and component regulating body by purifying a waste slurry containing silicon, comprising the steps of: preparing a mixture of silicon (Si), silicon carbide (SiC), water- A primary separation step of separating the water-soluble oil and the water from the initial waste slurry in a state where water is mixed with an initial waste slurry containing iron (Fe) at a first mixing ratio to obtain a Si-SiC-containing slurry; and And drying the Si-SiC-containing slurry, wherein the volume median diameter (Dv50) of the particles constituting the initial waste slurry is 1 占 퐉 or more.

The first mixing ratio is set so that the volume of the water is 0.2 to 8 times the volume of the initial waste slurry.

The method for manufacturing steelmaking steelmaking steel according to the present invention comprises mixing the Si-SiC-containing slurry obtained through the first separation step at a second mixing ratio, mixing the slurry, filtering the Si- Containing slurry is washed with an oil-cleaning step of cleaning the water-soluble oil remaining in the slurry.

The second mixing ratio is set so that the volume of the water is not less than 0.2 times and not more than 8 times the volume of the Si-SiC-containing slurry.

The method for producing steelmaking heat and component regulator according to the present invention is characterized in that after the primary separation step, the water-soluble oil and water separated from the initial waste slurry are fractionally distilled through the primary separation step, And a second separating step of separating the first separator and the second separator from each other.

In the first separation step, an initial waste slurry mixed and stirred with water is filtered by a pressing method to remove the water-soluble oil and the water from the initial waste slurry, .

In the first stage separation step, centrifugation is applied to an initial waste slurry mixed with water to separate the water-soluble oil and the water from the initial waste slurry .

In the present invention, the volume median diameter (Dv 50) of the particles constituting the initial waste slurry is limited to 1 탆 or more, Characterized in that the possibility of ignition due to the reaction of the fine particles of silicon with the oxygen and the oxidation amount of the silicon is reduced by reducing the fine powder component of the silicon and the total surface area of the silicon.

According to the present invention, there is provided a method for producing briquettes for controlling the heat and composition used in a steelmaking process by purifying a waste slurry containing silicon generated during the production of semiconductors or solar cell wafers, There is an effect that a method of manufacturing a sieve is provided.

The present invention also provides a method for manufacturing a briquette for controlling heat and composition for use in a steelmaking process capable of preventing the possibility of ignition due to the reaction of moisture with a silicon fine powder component that may occur during the reprocessing of a silicon- There is provided an effect of providing a method for manufacturing a steelmaking heat and composition regulating material which is a raw material.

Also, there is a method of manufacturing briquettes for controlling the heat and composition used in the steelmaking process which can effectively suppress the amount of silicon oxidation during the reprocessing of the silicon-containing waste slurry, and a method for preparing the briquetting heat- There is an effect that a manufacturing method is provided.

The present invention also relates to a method for producing a briquetting heat and composition controlling material used in a steelmaking process capable of preventing a molded briquette from being broken due to a decrease in the strength of the briquette which is a lumpy molded product, And a method for producing a component adjuster are provided.

In addition, the silicon-containing waste slurry, which is a factor of environmental pollution, is recycled and used as a briquetting heat for regenerating and controlling the components used in the steelmaking process without incineration or landfilling, thereby reducing waste treatment costs and ensuring cost competitiveness by cost reduction At the same time, there is an effect of minimizing environmental pollution that may occur in the steelmaking process.

Further, there is a method of manufacturing a briquetting heat and composition controlling breeze for use in an environmentally friendly steelmaking process by extracting and reusing the water-soluble oil contained in the silicon waste slurry and purifying discharged wastewater to a level that does not require reprocessing, There is provided an effect of providing a method for manufacturing a steelmaking heat and composition regulating material which is a raw material.

In addition, in the process of refining the silicon waste slurry, the amount of water to be mixed into the silicon waste slurry is optimized to improve the efficiency of briquetting for regenerating and regulating the composition, while reducing the reprocessing cost of discharged wastewater There is provided an effect of providing a method of manufacturing briquettes for regulating the heat and component used and a method of manufacturing a heat exchanger and component regulating body for steelmaking which are the raw materials of the briquetting.

In addition, a waste slurry containing silicon generated during the production of semiconductor or solar cell wafers is refined to prepare a powder, and a binder is added thereto to briquetize the briquettes for use in the process of manufacturing molten steel in the steelmaking process And a method of manufacturing a steelmaking heat and composition regulating material which is a raw material for the briquetting at low cost and high efficiency.

In addition, the silicon waste slurry which is a factor of environmental pollution is not incinerated or buried, and it is recycled and used for regenerating agent and ingredient control in the process of manufacturing molten steel in a steel making plant, thereby reducing waste disposal cost and cost reduction And at the same time, it is possible to minimize the environmental pollution that may occur in the steelmaking process.

In addition, the wastewater containing water-soluble oil and water generated in the pulverization process of silicon waste slurry is reused as an additive in the production of briquettes, thereby eliminating the need to reprocess the discharged wastewater, The present invention provides a method for manufacturing briquettes for use in heat treatment and component adjustment used in the process of manufacturing molten steel in a steelmaking process and a method for manufacturing environmentally friendly and economical products for steelmaking, .

In addition, since the silicon waste slurry is pulverized and molded into briquettes, it is easy to put into the converter in the steelmaking process, and the risk of fire or explosion due to the powder can be removed.

1 is a view for conceptually explaining a process of purifying waste slurry containing silicon discharged as a by-product in the process of manufacturing a semiconductor wafer or a solar cell wafer,
FIG. 2 is a process flow chart for explaining a method of purifying a waste slurry containing silicon according to an embodiment of the present invention to produce a briquetting heat and a briquetting agent for use in a steelmaking process,
3 is a view for explaining an example of a device configuration to which an embodiment of the present invention is applied,
FIG. 4 is a view for explaining an example of a specific configuration of the fractionation distillation system included in FIG. 3,
5 is a graph of an exemplary volume-based particle size distribution graph and volume-based cumulative particle size distribution for defining a volume median diameter (Dv50) of a particle group constituting a waste slurry in an embodiment of the present invention,
6 is a volume-based particle size distribution graph and a volume-based cumulative particle size distribution graph of particles constituting a waste slurry having a volume median diameter (Dv50) of 0.9774 m,
7 is a volume-based particle size distribution graph and a volume-based cumulative particle size distribution graph of particles constituting a waste slurry having a volume median diameter (Dv50) of 1.5683 m,
8 is a volume-based particle size distribution graph and a volume-based cumulative particle size distribution graph of particles constituting a waste slurry having a volume median diameter (Dv50) of 4.1155 占 퐉,
9 is a volume-based particle size distribution graph and volume-based cumulative particle size distribution graph of a particle group constituting a waste slurry having a volume median diameter (Dv50) of 7.0562 mu m,
10 is a volume-based particle size distribution graph and a volume-based cumulative particle size distribution graph of particles constituting a waste slurry having a volume median diameter (Dv50) of 9.6541 占 퐉,
11 is a volume-based particle size distribution graph and a volume-based cumulative particle size distribution graph of particles constituting a waste slurry having a volume median diameter (Dv50) of 11.9273 占 퐉.

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

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear.

FIG. 1 is a view for conceptually explaining a process of purifying a waste slurry containing silicon discharged as a by-product in the process of manufacturing a semiconductor wafer or a solar cell wafer.

Referring to FIG. 1, a waste slurry generated in a cutting step of a silicon ingot or a surface polishing step of a silicon wafer includes a fine powder such as cutting material, cutting oil, cutting oil, cutting material or wire saw, .

In order to separate the recoverable silicon and cutting material from such waste slurry, an oil cleaning process is performed as shown. Through this oil cleaning process, the cutting oil is removed, and the wastewater generated at this time is sent to the wastewater treatment system and recycled again. Meanwhile, the waste slurry that has been subjected to the oil cleaning process is separated and recycled into effective silicon through a silicon separation process. In this case, a centrifugation step may be performed to separate silicon. And the separated silicon is recycled through the drying process.

Since the silicon separated in the silicon separation process is separated and recycled, only the silicon having a large particle size is recycled. Therefore, the pulverized slurry after the separation of the large-particle silicon still contains a large amount of pulverized material, impurities, do.

FIG. 2 is a process flow chart for explaining a method of purifying waste slurries containing silicon according to an embodiment of the present invention to produce briquettes for controlling heat and composition used in a steelmaking process, and FIG. 3 is a flowchart 1 is a diagram for explaining an example of a device configuration to which an example is applied.

Referring to FIGS. 2 and 3, an embodiment of the present invention includes a primary separation step S10, a secondary separation step S20, an oil cleaning step S30, a drying step S40, a crushing step S50, And a briquetting molding step (S60).

Before describing each step constituting one embodiment of the present invention, an initial waste slurry, which is a substance to be purified, will be described.

The initial waste slurry before the purifying process according to an embodiment of the present invention is composed of particles having various diameters. When the content of the fine powder component is high, the following problems are encountered in the process of recycling for the steelmaking process Lt; / RTI > That is, in the drying process for recycling the initial waste slurry, there is a possibility of ignition due to the reaction between the silicon fine powder component and water. In addition, the increase in the silicon fine powder content causes an increase in the overall surface area of silicon, thereby increasing the silicon oxide amount because the contact area between silicon and oxygen is increased. Also, according to one embodiment of the present invention, the refined silicon-containing powder is processed into a briquette, which is a lumpy molded product for use in a steelmaking process, since the higher the silicon fine powder content, the lower the strength of the briquettes , There is a problem that the molded briquettes are easily broken.

In order to solve these problems, an embodiment of the present invention is to provide a waste slurry having a volume median diameter (Dv50) of 1 mu m or more based on an experiment on waste slurry samples having various particle distributions . That is, the volume median diameter of the particles constituting the waste slurry used in one embodiment of the present invention is limited to 1 탆 or more.

By limiting the size of the group of particles constituting the waste slurry in this manner, it is possible to prevent the possibility of ignition due to the reaction of the silicon fine powder component with moisture and effectively suppress the silicon oxidation having a tendency proportional to the silicon surface area, It is possible to prevent the briquetting of the molded briquettes due to the decrease in the strength of the briquette which is a lumpy molded product in the subsequent briquette forming process.

Hereinafter, the volume median diameter (Dv50) is defined with reference to FIG.

FIG. 5 is a graph of an exemplary volume-based particle size distribution graph and volume-based cumulative particle size distribution for defining a volume median diameter (Dv 50) of a particle group constituting a waste slurry in an embodiment of the present invention. Particle size analysis can be performed using a laser diffraction and scattering type particle size analyzer.

Reference numeral A in FIG. 5 is a volume-based particle size distribution graph of particles constituting the waste slurry. The abscissa of the volumetric particle size distribution graph is the particle size of the particle group (Particle Diameter, 탆), and the ordinate is the ratio of the particle group having a specific particle size to the entire volume. The volumetric particle size distribution graph shows the ratio of particle groups having a specific particle size to the total volume.

Reference numeral B in FIG. 5 is a volume-based cumulative particle size distribution graph of particles constituting the waste slurry. The abscissa of the volume-based cumulative particle size distribution graph is the particle diameter (탆) of the particle group, and the ordinate is the cumulative volume ratio accumulated from the volume ratio of the particle group having a large particle size. The volumetric cumulative particle size distribution graph shows the particle size of the smallest particle among the particles belonging to the particle group having a specific cumulative volume ratio.

The particle size of the smallest particle among the particles belonging to the particle group having the cumulative volume ratio of 50% is 7.425 탆, and this value is the volume median diameter (Dv50).

On the other hand, the particle size of the smallest particle among the particles belonging to the particle group having a cumulative volume ratio of 10% is 9.698 μm, and this value is named Dv10.

The particle size of the smallest particle among the particles belonging to the particle group having a cumulative volume ratio of 90% is 3.974 μm, and this value is named Dv 90.

Hereinafter, each step constituting one embodiment of the present invention will be described in detail with the assumption that the volume median diameter (Dv50) of the particle group constituting the waste slurry is 1 탆 or more.

The briquettes, which are the final product of the embodiment of the present invention, that is, the briquettes for controlling the heat and the components used in the process of manufacturing molten steel in the steelmaking process, can be manufactured through the primary separation step (S10) and the briquetting step (S60) Step S30, drying step S40 and crushing step S50 are optional. That is, it is found that at least one of the oil cleaning step S30, the drying step S40, and the crushing step S50 is a process that can be selectively performed in the briquetting process. Hereinafter, The brittle manufacturing process is performed on the basis of the case where the brittle forming step (S10), the secondary separating step (S20), the oil cleaning step (S30), the drying step (S40), the crushing step (S50) Will be described in detail.

First, in the primary separation step S10, silicon (Si), silicon carbide (SiC), water-soluble oil, The initial waste slurry containing iron (Fe) and copper (Cu) is mixed with water at a first mixing ratio, and then the water is separated from the initial waste slurry. When the primary separation step (S10) is carried out, the water-soluble oil and water are separated from the initial waste slurry, whereby a Si-SiC-containing slurry is obtained.

For example, the initial waste slurry may be a material containing silicon, which is generated as a by-product such as a wire sawing process in the process of manufacturing a semiconductor wafer or a solar cell wafer. When a semiconductor wafer or a process of manufacturing a solar cell wafer is performed, The size of the included silicon carbide (SiC) has some variation in its size. Therefore, before performing the first separating step S10 of the present embodiment, a process of separately separating silicon carbide (SiC) having a relatively large size may be performed through a centrifugal separation process or the like.

The waste slurry, which is a by-product of the wire-sawing process, contains water-soluble oil (for example, PEG + DEG) in an amount of 10 wt% to 30 wt% in small amounts. In the steel making process including the steelmaking process, This oil should be removed to a certain level in order to be used.

As a method for removing oil, a combustion method using high temperature and a cleaning method using water may be applied. However, according to the method of burning the oil using the high temperature, there is a problem that the higher the oil content, the more the air pollution becomes and the possibility of the oxidation of the silicon due to the high temperature is a problem. Further, according to the method of washing a waste slurry containing a large amount of water-soluble oil with water, there is a problem in that the waste water treatment cost is increased.

This embodiment is configured to primarily separate the water-soluble oil from the initial waste slurry, reuse it through the process described below, and, if necessary, perform a water-based cleaning process on the Si-SiC containing slurry in which the water- According to this configuration, air pollution and silicon oxidation due to oil combustion can be prevented, and water-soluble oil can be reused, which is advantageous in terms of economy. In addition, since water is separated from the water-soluble oil through fractional distillation as described later, there is an advantage that the treatment cost for the finally generated wastewater is hardly generated.

In addition, the separated water can be reused as the material contained in the binder added for manufacturing the briquettes.

For this purpose, in this embodiment, a water-soluble oil and water are separated from the initial waste slurry by applying a pressing method using, for example, a filter press or the like, in a state in which water is mixed with the initial waste slurry to such an extent that stirring and pumping are possible After that, water is evaporated to recycle the water-soluble oil, and the slurry containing the water-soluble oil at a certain level, that is, the Si-SiC-containing slurry, is dried and pulverized to an appropriate size and then molded into briquettes. It is used for heat control and ingredient control used in

An example of a specific configuration of the primary separation step S10 will be described below.

The primary separation step S10 may be configured to include steps S12, S14, and S16.

First, in step S12, the initial waste slurry stored in the waste slurry storage tank is supplied to the first agitator 10, and water corresponding to the first mixing ratio is supplied to the first agitator 10, Are mixed with each other.

For example, the interior of the spent slurry storage tank may be configured to maintain a constant temperature to prevent the viscosity of the initially stored waste slurry from decreasing. Also, in order to prevent the initial waste slurry being stored from hardening due to sedimentation over time, the waste slurry storage tank is configured to support the agitation function .

The initial waste slurry includes semiconductor wafers or by-products generated during the manufacturing process of the solar cell wafers, and specifically includes silicon (Si), silicon carbide (SiC), water soluble oil, iron (Fe), and copper can do.

The first mixing ratio of the initial waste slurry and water may be set in the range of 1: 0.2 to 1: 8 on a volume basis. That is, the water is mixed with the initial waste slurry so that the volume of water is 0.2 to 8 times the volume of the initial waste slurry. As described above, the first mixing ratio is set considering the agitation and pumping of the initial waste slurry.

In step S14, the first agitator 10 is operated to stir the waste slurry mixed with water.

In step S16, when the set agitation time has elapsed, a process of supplying the agitated waste slurry to the first filtering system 20 to separate water and the water-soluble oil from the initial waste slurry is performed. As a specific filtering method, for example, a method of separating water and water-soluble oil by applying a pressing method using a filter press may be applied, and various known techniques such as a centrifugal separation method may be applied in addition to this method.

When this filtering process is performed, the water-soluble oil contained in the initial waste slurry is removed to a certain level, and a Si-SiC-containing slurry is obtained.

As described above, the primary separation step (S10) can be configured to separate the water-soluble oil and water from the initial waste slurry by filtering the stirred initial slurry mixed with water and pressing it in a pressing manner. As another example, the primary separation step (S10) may be configured to separate water-soluble oil and water from the initial waste slurry by applying centrifugation to the initial waste slurry mixed with water.

On the other hand, as will be described later, when the Si-SiC-containing slurry, which is one of the intermediates produced according to this embodiment, is dried and pulverized, a Si-SiC-containing powder is obtained. Since this Si- There is a risk of fire if you put it directly into a converter. Therefore, the Si-SiC-containing powder is compressed and formed into a briquette in the form of a lump having a predetermined size and shape through the briquetting step (S60) to be described later. Here, if the amount of oil contained in the Si-SiC-containing powder, which is an intermediate material for producing briquetting for the purpose of heat and component conditioning, is too small, the shape of the pressed briquet can be broken without being retained, - The inclusion of a certain amount of oil component in the SiC-containing powder may be helpful in manufacturing briquettes. If the content of the water-soluble oil remaining in the Si-SiC-containing slurry obtained through the first separation step (S10) is excessively large, the water-soluble oil component is removed again to an appropriate level through an oil cleaning step (S30) do.

Next, in the secondary separation step (S20), a process of separating the water-soluble oil and the water from each other is performed by fractional distillation of the water-soluble oil and water separated from the initial waste slurry through the primary separation step (S10). The water-soluble oil extracted through this process is purified to a recyclable level, and the water is purified so that no additional wastewater treatment process is required.

Hereinafter, with reference additionally to FIG. 4, an example of a specific configuration of the fractionation distillation system 30 in which the secondary separation step S20 is performed will be described. The fractionation system 30 includes a water / oil storage tank 310, a pump 320, a distillation column 330, a first collecting means 340, a second collecting means 350, a first heat exchanger 360, A second heat exchanger 370, a water storage tank 380, and an oil storage tank 390.

The water-soluble oil and water separated from the initial waste slurry through the primary separation step (S10) are supplied to the water / oil storage tank 310 and temporarily stored.

Hereinafter, the case where the water-soluble oil is composed of PEG and DEG is described as an example. It should be noted that the numerical values, such as temperature, pressure, flow rate, etc., disclosed in the following description are merely examples, and are values that can be changed according to specific requirements.

In FIG. 4, for example, the temperature and pressure at specific points F, F1, F2, B1, B2, B3, W1, W2 and W3 at which the valves are installed, And the water-soluble oil and water stored in the water / oil storage tank 310 have a mixing ratio of PEG: DEG: water of 20:13:67 on a wt% basis.

The pump 320 supplies the water-soluble oil and water to the distillation tower 330 under the conditions of a temperature of 20 ° C, a pressure of 760 mmHg, and a flow rate of 300 kg / hr.

The distillation column 330 is a means for separating the water-soluble oil and water from each other by fractional distillation, and can be largely divided into a heating section, a cooling section and a collecting section functionally.

For example, the distillation column 330 may be configured to perform the distillation in multiple stages, i.e., in one example, 10 stages, and in a state where the boiler steam is fed to the reboiler at 150 ° C or higher, the first collecting means 340 is 51.5 ° C., the pressure is 100 mmHg, the water is 200 kg / hr, and the second collecting means 350 collects the water Is 137 DEG C, the pressure is 106 mmHg, and the flow rate is 99.5 Kg / hr, that is, PEG / DEG.

The water supplied by the first collecting means 340 is 51.5 ° C., the pressure is 100 mmHg and the flow rate is 200 kg / hr. The water is passed through the first heat exchanger 360 at a temperature of 30 ° C., a pressure of 2967 mmHg, Is supplied to the water storage tank 380 at a rate of 200 kg / hr.

The water-soluble oil supplied by the second collecting means 350 at a temperature of 137 占 폚, a pressure of 106 mmHg and a flow rate of 99.5 kg / hr was passed through the second heat exchanger 370 at a temperature of 30 占 폚, a pressure of 2967 mmHg And supplied to the oil storage tank 390 at a flow rate of 99.5 Kg / hr.

The water storage tank 380 is a means for storing water supplied through the first heat exchanger 360. The temperature of water to be stored is 30 ° C and the pressure is 760 mmHg. As a result of the simulation, the COD is only a few ppm It was found that the waste water treatment was not necessary.

The oil storage tank 390 is a means for storing the oil supplied through the second heat exchanger 370. The temperature of the oil to be stored is 30 DEG C and the pressure is 760 mmHg. As a result of the simulation, %, PEG was 60.3 wt%, and DEG was 39.2 wt%.

Next, in the oil cleaning step (S30), the slurry in which the water-soluble oil and water are separated through the primary separation step (S10) is mixed with the Si-SiC containing slurry in the second mixing ratio Followed by washing the water-soluble oil remaining in the Si-SiC-containing slurry.

For example, the second mixing ratio may be set so that the volume of water is no less than 0.2 times and no more than 8 times the volume of the Si-SiC containing slurry, and the oil cleaning step S30 is configured to be performed at a low temperature of 50 DEG C or lower .

As described above, although the water-soluble oil contained in the initial waste slurry is removed at a certain level through the primary separation step (S10), it may be necessary to further remove the remaining water-soluble oil according to the process conditions and the like. The process is an oil cleaning step (S30).

An example of the specific configuration of the oil cleaning step S30 will be described below.

The oil cleaning step S30 may be configured to include steps S32, S34, and step S36.

First, in step S32, the slurry in which the water-soluble oil is separated and removed to a certain level through the first separation step (S10) is supplied to the second agitator 40, and the slurry containing the Si- Water is supplied to the second agitator 40, whereby a process of mixing water into the Si-SiC-containing slurry is performed.

The second mixing ratio of the Si-SiC-containing slurry and water may be set in the range of 1: 0.2 to 1: 8 on a volume basis. That is, water is mixed with the Si-SiC-containing slurry so that the volume of water is 0.2 times or more and 8 times or less the volume of the slurry containing Si-SiC.

The reason why the mixing ratio of the Si-SiC-containing slurry and water is set as described above is as follows.

When the mixing ratio is less than 0.2, it is difficult to carry out the subsequent stirring process and pumping process in consideration of the viscosity of the Si-SiC-containing slurry. When the mixing ratio is more than 8 times, the removal rate of the water-soluble oil is drastically increased, Which may cause difficulties in the process of briquetting (S60)

That is, the water mixed in the Si-SiC-containing slurry is combined with the water-soluble oil through the stirring and filtering processes to be described later and discharged to the outside in the form of wastewater. This wastewater may be an environmental pollutant, so it is subjected to additional wastewater treatment. Considering this, it is recommended to increase the amount of water to facilitate wastewater treatment. Also, as the amount of water is increased, the amount of oil removed from the Si-SiC-containing slurry is increased because the oil level is increased.

On the other hand, as described above, the Si-SiC-containing powder is obtained by drying and pulverizing the Si-SiC-containing slurry, which is one of the intermediates produced according to the present embodiment, Therefore, there is a risk of occurrence of fire when it is directly supplied to a converter (convertor). Therefore, the Si-SiC-containing powder is compressed and formed into a briquette in the form of a lump having a predetermined size and shape through the briquetting step (S60) to be described later. Here, if the amount of the oil contained in the Si-SiC-containing powder, which is the raw material for producing the briquetting for the purpose of heat treatment and component conditioning, is excessively small, the shape of the pressed briquet can be broken without being retained, The SiC-containing powder preferably contains a certain amount of an oil component.

Therefore, in order to improve the efficiency of wastewater treatment and briquetting, the mixing ratio of the Si-SiC-containing powder and water was set as described above.

Next, in S14, a process of promoting the dissolution of the water-soluble oil remaining in the Si-SiC-containing slurry is performed by operating the second agitator 40 to stir the Si-SiC-containing slurry in which the water is mixed.

Next, in step S16, when the set stirring time has elapsed, the Si-SiC-containing slurry stirred with water is supplied to the second filtering system 50 to remove water and the water-soluble oil dissolved in the water from the Si- A process of filtering and removing is performed. The specific filtering scheme may be configured by applying various known techniques.

On the other hand, in the process of cleaning the slurry containing Si-SiC with water, if the water temperature is too low, five days cleaning power of a number can be lowered, and the water temperature is high, silicon dioxide and silicon are reacted with water (SiO ₂₎ is created, And the heat generation characteristics can be lowered. Therefore, in order to prevent such a problem, this embodiment can be configured so that the entire process or some processes of the oil cleaning step S30 are performed at a low temperature of 50 DEG C or less.

Next, in the drying step (S40), a process of supplying the slurry containing Si-SiC, in which the water-soluble oil has been washed through the oil cleaning step (S30), to the dryer (60) and drying at a set drying temperature is performed. The drying step (S40) may be selectively performed as required, and may be performed in a natural drying method, or in an atmospheric air or a nitrogen atmosphere at 200 DEG C or less.

An example of a concrete configuration of the drying step S40 will be described below.

The drying step (S40) is a step of drying the Si-SiC-containing slurry in which the water-soluble oil has been removed to a certain level, before pulverizing.

Here, when the silicon contained in the Si-SiC-containing slurry is exposed to the atmospheric state for a certain period of time, the silicon oxide is generated by the oxygen present in the atmosphere, and therefore the heat generation characteristics of the heat-transfer agent may be deteriorated.

Therefore, in order to prevent such a problem, the present embodiment is configured to perform the Si-SiC-containing slurry drying process at a low temperature of 200 占 폚 or less, more specifically, 110 占 폚 to 130 占 폚 in an atmospheric atmosphere or a nitrogen atmosphere. When the Si-SiC-containing slurry is dried in a nitrogen atmosphere, since the drying temperature can be raised to a high temperature without oxidation of silicon, the drying speed is increased and the drying rate is increased.

In the pulverization step (S50), the slurry containing Si-SiC in the form of a lump dried in the drying step (S40) is supplied to the pulverizer (70) and pulverized. This pulverization step (S50) can be optionally carried out as needed.

For example, in the pulverization step (S50), the dried Si-SiC-containing slurry may be configured to be pulverized into powders having a diameter of 5 cm or less. After the pulverization step (S50), one of the intermediate products of this embodiment Si-SiC < / RTI > containing powder is obtained, which powder may have any regular or irregular shape.

Next, in the briquetting step S60, a binder is added to the Si-SiC-containing powder obtained through the pulverization step (S50), and after stirring, the briquette is formed by using the briquetting machine 80, Is performed.

An example of a concrete configuration of the brittle forming step S60 will be described below.

The briquetting molding step S60 may be configured to include steps S62, S64 and S66.

In step S62, a process of adding an iron component (Fe source) and a binder to the Si-SiC-containing powder obtained through the pulverization step (S50) is performed.

The addition of the iron component is optional, and one of the reasons for adding the iron component is to control the weight of the finally produced briquettes. That is, the briquettes for the purpose of heat treatment and component adjustment, which are final products manufactured according to the present embodiment, are put into the converter during the process of manufacturing molten steel in the steelmaking process. If the specific gravity of the briquets is too low, The molten steel does not penetrate into the molten steel of the molten steel and floats on the surface thereof.

To prevent this, the present embodiment adds an iron component to the Si-SiC-containing powder, and in this embodiment, the addition of the iron component is optional.

For example, when the iron component is further added to the Si-SiC-containing slurry in the briquetting step S60, the slurry containing Si-SiC is 30 wt% or more and the iron component is 30 wt% or more, Or less.

Examples of specific weight composition ratios for the case where the iron component is added and the case where the iron component is not added are as follows.

That is, for example, the Si-SiC-containing slurry may be set to 30 wt% or more, the iron component may be 50 wt% or less, and the other components including the binder may be 3 wt% or more and 15 wt% or less based on the weight of the briquettes . SiC-containing slurry may be used only in the steelmaking process without adding an iron component. In this case, however, since the binder is used for producing the briquettes, the maximum weight composition ratio of the Si-SiC containing slurry is about 97% Can be set.

The binder added in step S62 is to make the Si-SiC-containing powder or the Si-SiC-Fe-containing powder have a certain viscosity for briquet molding, and is preferably made of molasses, starch, bentonite, And one or more members selected from the group consisting of water and a water-soluble oil.

The mixing ratio between the material components constituting the binder may vary depending on the situation, and the binder may be mixed with water, water-soluble oil may be mixed, or water-soluble oil may be mixed with water.

For example, when water is mixed with the binder, water separated from the water-soluble oil through the secondary separation step (S20) can be reused as a material contained in the binder. In this case, some of the Si is oxidized to SiO ₂ , which may cause a problem of lowering the efficiency of the briquetting device for endothermic and component adjustment purposes as the final product. When water is used in combination with the binder, it is preferable to mix the minimum quantity of water in the shortest time for briquetting in order to prevent oxidation of Si.

In step S64, stirring is performed so that the constituents of the Si-SiC-containing powder or the Si-SiC-Fe-containing powder to which the binder is added are appropriately mixed. Of course, for this stirring, the briquetting machine 80 may be configured to support the self-stirring function or may be stirred using a separate stirrer.

In Step S66, a process of molding the Si-SiC-containing powder or the Si-SiC-Fe-containing powder added with the binder and stirring is molded into the briquettes having a specific shape by using the briquetting machine 80.

Hereinafter, the experiment for deriving the first mixing ratio titration range in the primary separation step (S10) for each volume median diameter (Dv50) of the particle group constituting the waste slurry and the results of this experiment are shown in Tables 1 to 6 below . The waste slurry in which the oil has been removed to a certain level through the primary separation step (S10) is referred to as Si-SiC-containing slurry. This Si-SiC-containing slurry is a material containing silicon (Si), silicon carbide (SiC), and an oil whose content is below a certain level. In addition, the Si-SiC-containing slurry may additionally contain metal components such as iron (Fe) which is a wire saw wear component. The Si-SiC-containing slurry is subjected to a drying step (S40) and a pulverization step (S50) to form a Si-SiC-containing powder.

In this experiment, particle size analysis of the waste slurry was performed using HORIBA LA-300, a laser diffraction and scattering type particle size analyzer, and the amount of oil contained in the Si-SiC-containing powder was measured after separating the oil component , And the content of oxygen contained in the Si-SiC-containing powder was measured using a WD-XRF spectrometer. The content of oxygen contained in the Si-SiC-containing powder is an index for estimating the oxidation amount of silicon.

Table 1 shows experimental results for waste slurries having a volume median diameter (Dv 50) of 0.9774 μm, and FIG. 6 is a graph showing the results of experiments on particle groups constituting a waste slurry having a volume median diameter (Dv 50) of 0.9774 μm A volumetric particle size distribution graph and a volumetric cumulative particle size distribution graph.

division The first mixing ratio (water / waste slurry) Drying time (hour) Drying temperature (캜) Oil content (wt%) Oxygen content (wt%) Experimental Example 1 0.10 8 120 3.23 7.26546 Experimental Example 2 0.15 8 120 3.12 7.23219 Experimental Example 3 0.20 8 120 3.26 7.46943 Experimental Example 4 0.25 8 120 3.44 7.56987 Experimental Example 5 1.00 8 120 3.21 7.16546 Experimental Example 6 2.00 8 120 2.34 7.63216 Experimental Example 7 3.00 8 120 2.11 7.26540 Experimental Example 8 4.00 8 120 1.68 7.30168 Experimental Example 9 5.00 8 120 1.55 7.10111 Experimental Example 10 6.00 8 120 1.24 7.53540 Experimental Example 11 7.00 8 120 1.03 7.66840 Experimental Example 12 7.50 8 120 0.85 7.93216 Experimental Example 13 8.00 8 120 0.65 7.96989 Experimental Example 14 8.50 8 120 0.74 7.66596

Referring to Table 1 and FIG. 6, when the volume median diameter (Dv50) of the particle group constituting the waste slurry is 0.9774 탆, the amount of silicon fine particles contained in the waste slurry is excessively large, The ignition occurred. The reason for the extremely low oil content in Table 1 is that the oil burned due to ignition during the drying process. From these experimental results, it can be seen that waste sludge having a Dv 50 of less than 1 탆 is not suitable for manufacturing briquettes.

Table 2 shows experimental results of the waste slurry having a volume median diameter (Dv 50) of 1.5683 μm of the constituent particles, and FIG. 7 is a graph showing the experimental results of the particle groups constituting the waste slurry having a volume median diameter (Dv 50) A volumetric particle size distribution graph and a volumetric cumulative particle size distribution graph.

division The first mixing ratio (water / waste slurry) Drying time (hour) Drying temperature (캜) Oil content (wt%) Oxygen content (wt%) Experimental Example 1 0.10 8 120 14.65 4.60166 Experimental Example 2 0.15 8 120 14.21 4.30686 Experimental Example 3 0.20 8 120 14.12 4.51066 Experimental Example 4 0.25 8 120 13.85 4.68403 Experimental Example 5 1.00 8 120 7.23 4.24987 Experimental Example 6 2.00 8 120 3.25 4.51089 Experimental Example 7 3.00 8 120 2.48 4.68403 Experimental Example 8 4.00 8 120 1.65 4.89806 Experimental Example 9 5.00 8 120 1.01 4.54608 Experimental Example 10 6.00 8 120 0.98 4.80169 Experimental Example 11 7.00 8 120 0.65 4.80191 Experimental Example 12 7.50 8 120 0.73 4.31659 Experimental Example 13 8.00 8 120 0.51 4.51094 Experimental Example 14 8.50 8 120 0.43 4.69870

Referring to Table 2 and FIG. 7, when the volume median diameter (Dv50) of the constituent particles constituting the waste slurry was 1.5683 占 퐉, no fire occurred during the drying process. In the first separation step (S10), when the first mixing ratio is 1, the oil starts to be significantly removed, and when the first mixing ratio is 8 times, the oil is sufficiently removed and the first mixing ratio is 0.1 to 8 times It can be confirmed that the oxygen content is at a level to be tolerated.

Table 3 shows experimental results of the waste slurry having a volume median diameter (Dv 50) of 4.1155 μm of the constituent particles, and FIG. 8 is a graph showing the results of experiments of the particle groups constituting the waste slurry having a volume median diameter (Dv 50) A volumetric particle size distribution graph and a volumetric cumulative particle size distribution graph.

division The first mixing ratio (water / waste slurry) Drying time (hour) Drying temperature (캜) Oil content (wt%) Oxygen content (wt%) Experimental Example 1 0.10 8 120 15.32 4.01354 Experimental Example 2 0.15 8 120 15.26 4.34984 Experimental Example 3 0.20 8 120 15.11 4.11341 Experimental Example 4 0.25 8 120 14.91 3.81093 Experimental Example 5 1.00 8 120 7.95 4.21097 Experimental Example 6 2.00 8 120 3.88 4.19409 Experimental Example 7 3.00 8 120 2.71 4.03498 Experimental Example 8 4.00 8 120 1.85 4.34609 Experimental Example 9 5.00 8 120 1.32 3.91673 Experimental Example 10 6.00 8 120 1.01 3.99840 Experimental Example 11 7.00 8 120 0.53 4.04987 Experimental Example 12 7.50 8 120 0.43 4.01894 Experimental Example 13 8.00 8 120 0.41 3.88471 Experimental Example 14 8.50 8 120 0.50 4.03984

Referring to Table 3 and FIG. 8, when the volume median diameter (Dv50) of the constituent particles constituting the waste slurry was 4.1155 탆, no fire occurred during the drying process. In the first separation step (S10), when the first mixing ratio is 1, the oil starts to be significantly removed, and when the first mixing ratio is 8 times, the oil is sufficiently removed and the first mixing ratio is 0.1 to 8 times It can be confirmed that the oxygen content is at a level to be tolerated.

Table 4 shows experimental results of waste slurries having a volume median diameter (Dv 50) of 7.0562 μm, and FIG. 9 is a graph showing the results of experiments on particle groups constituting a waste slurry having a volume median diameter (Dv 50) of 7.0562 μm A volumetric particle size distribution graph and a volumetric cumulative particle size distribution graph.

division The first mixing ratio (water / waste slurry) Drying time (hour) Drying temperature (캜) Oil content (wt%) Oxygen content (wt%) Experimental Example 1 0.10 8 120 14.76 3.81850 Experimental Example 2 0.15 8 120 14.61 3.76549 Experimental Example 3 0.20 8 120 14.53 3.66406 Experimental Example 4 0.25 8 120 13.89 3.78008 Experimental Example 5 1.00 8 120 6.88 3.84098 Experimental Example 6 2.00 8 120 3.23 3.80498 Experimental Example 7 3.00 8 120 2.22 3.54893 Experimental Example 8 4.00 8 120 1.69 3.64089 Experimental Example 9 5.00 8 120 0.82 3.61801 Experimental Example 10 6.00 8 120 0.43 3.78764 Experimental Example 11 7.00 8 120 0.22 3.59841 Experimental Example 12 7.50 8 120 0.21 3.89804 Experimental Example 13 8.00 8 120 0.00 3.68400 Experimental Example 14 8.50 8 120 0.00 3.71509

Referring to Table 4 and FIG. 9, when the volume median diameter (Dv50) of the constituent particles constituting the waste slurry was 7.0562 占 퐉, no fire occurred during the drying process. In the first separation step (S10), when the first mixing ratio is 1, the oil starts to be significantly removed, the oil is completely removed when the first mixing ratio is 8, and the first mixing ratio is 0.1 to 8 times It can be confirmed that the oxygen content is at a level to be tolerated.

Table 5 shows experimental results of the waste slurry having a volume median diameter (Dv 50) of 9.6541 μm of the constituent particles, and FIG. 10 is a graph showing the results of experiments of the particle groups constituting the waste slurry having a volume median diameter (Dv 50) of 9.6541 μm A volumetric particle size distribution graph and a volumetric cumulative particle size distribution graph.

division The first mixing ratio (water / waste slurry) Drying time (hour) Drying temperature (캜) Oil content (wt%) Oxygen content (wt%) Experimental Example 1 0.10 8 120 15.01 3.19483 Experimental Example 2 0.15 8 120 14.92 3.02409 Experimental Example 3 0.20 8 120 14.83 3.13108 Experimental Example 4 0.25 8 120 14.01 3.29413 Experimental Example 5 1.00 8 120 7.00 3.39844 Experimental Example 6 2.00 8 120 4.03 3.39781 Experimental Example 7 3.00 8 120 2.56 3.24903 Experimental Example 8 4.00 8 120 1.85 3.29873 Experimental Example 9 5.00 8 120 1.11 3.29841 Experimental Example 10 6.00 8 120 0.86 3.05997 Experimental Example 11 7.00 8 120 0.65 3.26987 Experimental Example 12 7.50 8 120 0.60 3.39840 Experimental Example 13 8.00 8 120 0.33 3.19847 Experimental Example 14 8.50 8 120 0.32 3.19840

Referring to Table 5 and FIG. 10, when the volume median diameter (Dv50) of the constituent particles constituting the waste slurry was 9.6541 占 퐉, no fire occurred during the drying process. In the first separation step (S10), when the first mixing ratio is 1, the oil starts to be significantly removed, and when the first mixing ratio is 8 times, the oil is sufficiently removed and the first mixing ratio is 0.1 to 8 times It can be confirmed that the oxygen content is at a level to be tolerated.

Table 6 shows the experimental results of the waste slurry having the volume median diameter (Dv50) of 11.9273 占 퐉 of the constituent particles, and Fig. 11 shows the results of the experimental results of the particle groups constituting the waste slurry having the volume median diameter (Dv50) of 11.9273 占A volumetric particle size distribution graph and a volumetric cumulative particle size distribution graph.

division The first mixing ratio (water / waste slurry) Drying time (hour) Drying temperature (캜) Oil content (wt%) Oxygen content (wt%) Experimental Example 1 0.10 8 120 15.68 2.71353 Experimental Example 2 0.15 8 120 15.49 2.85465 Experimental Example 3 0.20 8 120 15.51 2.71101 Experimental Example 4 0.25 8 120 14.56 2.65103 Experimental Example 5 1.00 8 120 8.64 2.61098 Experimental Example 6 2.00 8 120 4.23 2.89458 Experimental Example 7 3.00 8 120 2.88 2.40564 Experimental Example 8 4.00 8 120 2.01 2.89878 Experimental Example 9 5.00 8 120 1.35 2.63156 Experimental Example 10 6.00 8 120 0.92 2.58406 Experimental Example 11 7.00 8 120 0.64 2.79873 Experimental Example 12 7.50 8 120 0.55 2.55040 Experimental Example 13 8.00 8 120 0.21 2.61094 Experimental Example 14 8.50 8 120 0.00 2.60463

Referring to Table 6 and FIG. 11, when the volume median diameter (Dv50) of the constituent particles constituting the waste slurry was 11.9273 占 퐉, no fire occurred during the drying process. In the first separation step (S10), when the first mixing ratio is 1, the oil starts to be significantly removed, and when the first mixing ratio is 8 times, the oil is sufficiently removed and the first mixing ratio is 0.1 to 8 times It can be confirmed that the oxygen content is at a level to be tolerated.

According to the experimental results shown in Tables 1 to 6, it can be confirmed that the volume median diameter (Dv50) of the constituent particles constituting the waste slurry is preferably 1 占 퐉 to 12 占 퐉.

When the volumetric median diameter (Dv50) of the constituent particles constituting the waste slurry is limited to 1 탆 or more and 12 탆 or less, in the process of removing the oil contained in the waste slurry and drying, It is possible to effectively suppress the silicon oxidation having a tendency proportional to the silicon surface area and to prevent the molded briquettes from being broken due to the decrease in the strength of the briquettes, The phenomenon can be prevented.

Further, according to the experimental results shown in Tables 1 to 6, when both the oil content and the oxygen content are considered, the fact that the first mixing ratio in the first separation step (S10) is preferably 0.2 to 8 times Can be confirmed.

The method for manufacturing steelmaking heat and component regulating body according to an embodiment of the present invention is a method for manufacturing a steelmaking heat and component regulating body by purifying a waste slurry containing silicon, , A water-soluble oil, and iron (Fe) in a first mixing ratio, and separating the water-soluble oil and the water from the initial waste slurry to obtain a Si-SiC-containing slurry And a drying step of drying the Si-SiC-containing slurry, wherein a volume median diameter (Dv50) of the particles constituting the initial waste slurry is 1 m or more.

Since the method for manufacturing steelmaking heat and component regulating body according to an embodiment of the present invention is a part of the method for manufacturing briquettes for controlling the heat and component used in the steelmaking process according to the embodiment of the present invention described in detail above, It is omitted.

As described above in detail, according to the present invention, there is provided a method of manufacturing a briquetting briquetting apparatus for purifying a waste slurry containing silicon generated during the manufacture of semiconductor or solar cell wafers, There is provided an effect of providing a method of manufacturing a steelmaking heat exchanger and a component adjusting body.

The present invention also provides a method for manufacturing a briquette for controlling heat and composition for use in a steelmaking process capable of preventing the possibility of ignition due to the reaction of moisture with a silicon fine powder component that may occur during the reprocessing of a silicon- There is provided an effect of providing a method for manufacturing a steelmaking heat and composition regulating material which is a raw material.

Also, there is a method of manufacturing briquettes for controlling the heat and composition used in the steelmaking process which can effectively suppress the amount of silicon oxidation during the reprocessing of the silicon-containing waste slurry, and a method for preparing the briquetting heat- There is an effect that a manufacturing method is provided.

The present invention also relates to a method for producing a briquetting heat and composition controlling material used in a steelmaking process capable of preventing a molded briquette from being broken due to a decrease in the strength of the briquette which is a lumpy molded product, And a method for producing a component adjuster are provided.

In addition, the silicon-containing waste slurry, which is a factor of environmental pollution, is recycled and used as a briquetting heat for regenerating and controlling the components used in the steelmaking process without incineration or landfilling, thereby reducing waste treatment costs and ensuring cost competitiveness by cost reduction At the same time, there is an effect of minimizing environmental pollution that may occur in the steelmaking process.

Further, there is a method of manufacturing a briquetting heat and composition controlling breeze for use in an environmentally friendly steelmaking process by extracting and reusing the water-soluble oil contained in the silicon waste slurry and purifying discharged wastewater to a level that does not require reprocessing, There is provided an effect of providing a method for manufacturing a steelmaking heat and composition regulating material which is a raw material.

In addition, in the process of refining the silicon waste slurry, the amount of water to be mixed into the silicon waste slurry is optimized to improve the efficiency of briquetting for regenerating and regulating the composition, while reducing the reprocessing cost of discharged wastewater There is provided an effect of providing a method of manufacturing briquettes for regulating the heat and component used and a method of manufacturing a heat exchanger and component regulating body for steelmaking which are the raw materials of the briquetting.

In addition, a waste slurry containing silicon generated during the production of semiconductor or solar cell wafers is refined to prepare a powder, and a binder is added thereto to briquetize the briquettes for use in the process of manufacturing molten steel in the steelmaking process And a method of manufacturing a steelmaking heat and composition regulating material which is a raw material for the briquetting at low cost and high efficiency.

In addition, the silicon waste slurry which is a factor of environmental pollution is not incinerated or buried, and it is recycled and used for regenerating agent and ingredient control in the process of manufacturing molten steel in a steel making plant, thereby reducing waste disposal cost and cost reduction And at the same time, it is possible to minimize the environmental pollution that may occur in the steelmaking process.

In addition, the wastewater containing water-soluble oil and water generated in the pulverization process of silicon waste slurry is reused as an additive in the production of briquettes, thereby eliminating the need to reprocess the discharged wastewater, The present invention provides a method for manufacturing briquettes for use in heat treatment and component adjustment used in the process of manufacturing molten steel in a steelmaking process and a method for manufacturing environmentally friendly and economical products for steelmaking, .

In addition, since the silicon waste slurry is pulverized and molded into briquettes, it is easy to put into the converter in the steelmaking process, and the risk of fire or explosion due to the powder can be removed.

While the present invention has been described in connection with what is presently considered to be preferred embodiments, it is to be understood that the invention is not limited to the disclosed embodiments. Further, it is obvious that various modifications can be made without departing from the scope of the technical idea of the present invention by anyone having ordinary skill in the art.

10: First stirrer
20: first filtering system
30: fractional distillation system
40: Second stirrer
50: second filtering system
60: dryer
70: crusher
80: Briquetting machine
310: Water / oil storage tank
320: pump
330: Distillation tower
340: first collecting means
350: Second collecting means
360: first heat exchanger
370: second heat exchanger
380: Water storage tank
390: Oil storage tank
S10: Primary separation step
S20: Secondary Separation Phase
S30: Oil rinsing step
S40: drying step
S50: crushing step
S60: Briquette forming step

Claims (20)

A method for producing a briquette for controlling heat and composition for use in the process of manufacturing molten steel in a steelmaking process by purifying a waste slurry containing silicon,
Separating said water-soluble oil and said water from said initial waste slurry in a first mixing ratio of water to an initial waste slurry comprising silicon (Si), silicon carbide (SiC), water-soluble oil and iron (Fe) A primary separation step; And
A briquetting step of adding a binder to the Si-SiC-containing slurry obtained by separating the water-soluble oil and the water from the initial waste slurry through the primary separation slurry, stirring the slurry, and molding the slurry into a briquette Including,
The volume median diameter (Dv50) of the particles constituting the initial closed slurry is limited to not less than 1 占 퐉 to reduce the fine powder component of the silicon contained in the waste slurry and the total surface area of the silicon, To reduce the possibility of ignition due to the reaction of oxygen with the differential component of the briquettes and to reduce the oxidation amount of the silicon. The method according to claim 1,
Wherein the first mixing ratio is set so that the volume of the water is at least 0.2 times and not more than 8 times the volume of the initial waste slurry. The method according to claim 1,
After the primary separation step and before the briquetting step,
An oil cleaning step of mixing the water with the Si-SiC-containing slurry obtained through the primary separation step in a mixed state at a set second mixing ratio, and then filtering and filtering the water-soluble oil remaining in the Si-SiC-containing slurry Wherein the briquetting step further comprises the step of heating the briquettes. The method of claim 3,
Wherein the second mixing ratio is set so that the volume of the water is not less than 0.2 times and not more than 8 times the volume of the Si-SiC containing slurry. The method according to claim 1,
And a secondary separation step of separating the water-soluble oil and the water from each other by fractional distillation of the water-soluble oil and water separated from the initial spent slurry through the primary separation step after the primary separation step Of the briquettes for regeneration and component control for use in the steelmaking process. The method according to claim 1,
Further comprising a drying step of drying the Si-SiC-containing slurry obtained through the primary separation step, before the briquetting step, in a steelmaking process. The method according to claim 6,
Characterized by further comprising a grinding step of grinding the dried Si-SiC-containing slurry through the drying step to obtain a Si-SiC-containing powder before the briquetting step, Method of manufacturing briquettes. 8. The method of claim 7,
Wherein the diameter of the Si-SiC-containing powder obtained through the pulverizing step is 5 cm or less. The method according to claim 1,
In the briquetting step, an Fe component is further added to the Si-SiC containing slurry,
Wherein the Si-SiC-containing slurry is not less than 30 wt% and the iron component is not more than 30 wt% based on the weight of the briquettes. The method according to claim 1,
In the primary separation step,
Wherein the initial waste slurry mixed with water and stirred is filtered in a pressing manner to separate the water-soluble oil and the water from the initial waste slurry. The method according to claim 1,
In the primary separation step,
A method of manufacturing briquettes for controlling heat and composition for use in a steelmaking process, characterized in that centrifugation is applied to an initial waste slurry mixed with water to separate said water-soluble oil and said water from said initial waste slurry. delete delete delete delete delete delete delete delete delete

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