KR101134230B1 - Purification method and system of chlorosilane, and purifying material for filtering metal impurities - Google Patents

Abstract

PURPOSE: A method and a system for refining chlorosilane and absorbent for eliminating metal-based impurities are provided to absorb and eliminate metal-based impurities from chlorosilane based on yellow soil-based absorbent. CONSTITUTION: A mixture contains 100-50 weight% of yellow soil powder and 0-50 weight% of a micropore formation aiding agent. The mixture is particulated and sintered to prepare absorbent(30) for eliminating metal-based impurities. An absorbent bed(18) is filled with the absorbent. Chlorosilane passes through the absorbent bed such that metal-based impurities contained in the chlorosilane is filtered by the absorbent. The micropore formation aiding agent contains at least one selected from kaolin, charcoal powder, and anion powder.

Description

Purification Method and System of Chlorinated Chloride and Adsorbent for Purifying Metallic Impurities {Purification Method and System of Chlorosilane, and Purifying Material for Filtering Metal Impurities}

The present invention relates to a technique for manufacturing a photovoltaic or semiconductor grade (hereinafter referred to as "electronic grade") chloride silane compounds (for example, silane trichloride, silicon tetrachloride, etc.), more specifically, an adsorbent having an ocher component. To remove metal-based impurities contained in silane chloride compounds such as silane trichloride, silicon tetrachloride, etc. to produce highly purified electronic grade trichlorosilane and / or silicon tetrachloride and purification systems, and to provide essential functions for such purification. It relates to an adsorbent for purifying metallic impurities.

It is known to use industrial trichlorosilane or monosilane as a raw material for producing electronic grade polysilicon. Trichlorosilane is prepared by reacting metal-grade silicon (called Metallurgical Silicon or MG-Si) and hydrogen chloride (HCl) in a fluidized bed reactor (called a fluidized bed reactor or FBR). The trichlorosilane produced contains a metal chloride component by the reaction of a metal impurity contained in the MG-Si component and chlorine gas (Cl ₂ ). Such metal impurities are metal components such as boron, phosphorus, arsenic, and the like, and they exist in the form of boron trichloride, phosphorus trichloride, arsenic trichloride, and the like. Trichloride silanes containing such impurities are not suitable for use in the manufacture of silicon wafers for semiconductors that precisely control electrical resistance control at concentrations of impurities. Therefore, the electronic grade chloride silane used to manufacture polysilicon by Chemical Vapor Deposition (CVD) is prepared through the process of purifying the metal impurities contained in the chloride silane produced in the fluidized bed reactor to 1ppbw or less. .

Conventional techniques for removing metal impurities contained in chlorosilanes are known by using a multi-stage distillation column to remove them using a separation column according to the boiling point of metal impurities or by physical methods using silica gel or activated carbon. have. These prior arts are mainly used to produce trichlorosilane and / or monosilane for solar and semiconductors.

As is well known, in order to remove metal impurities using a multi-stage distillation column (US Patent Nos. 4340574, 4676967, US Patent Application Publication No. 20028167), high purity chlorinated silane can be obtained. However, it may be difficult to obtain high purity silane chloride due to the temperature conditions of the distillation column or other operating conditions.

On the other hand, Japanese Patent Application Laid-Open No. 2001-131187 discloses a method for obtaining purified monosilane by contacting monosilane prepared by disproportionating alkoxysilane as a raw material with pure water. However, the impurities to be treated in this method are hydrocarbons.

In addition, Korean Patent Publication No. 10-0795963 discloses a method for removing boron and phosphorus-based metal impurities by a monosilane purification method of washing monosilane at a pH of 7 to 10 and drying it with an absorbent. However, if the water removal is not smooth in this method, there is a problem that other compounds are prepared by the reaction of silanes and water.

On the other hand, Korean Patent Publication Nos. 10-0981813 and US Patent No. 7879198 B2 propose a method of effectively removing metal impurities by varying boiling points by chemically inducing bonding with boron and phosphorus compounds. However, in this method, it is difficult to quantitatively control the chemical compound with the metal compound, and when the concentration is high, the removal is difficult.

The present invention was derived in view of the problems of the prior art as described above, an object of the present invention is to include in the silane chloride to prepare an electronic grade silane from chlorine silane separated through a multi-stage distillation column in the process of purifying chlorine silane. The present invention provides a method for secondary purification using high purity pure chlorine chloride by adsorbing and removing a metal-based impurity using an adsorbent composed mainly of ocher, and a silane chloride purification system for the same.

Another object of the present invention is to provide an adsorbent for purifying metallic impurities which plays a key role in such secondary purification of silane chloride.

In order to achieve the above object, according to an aspect of the present invention, in the purification of the silane chloride, using a mixture containing 100 to 50% by weight of the ocher powder and 0 to 50% by weight of the microporous forming aids of a predetermined form Chlorinated silane is passed through an adsorptive bed filled with particles of a metal-based impurity refining adsorbent, and the metal impurities contained in the chlorosilane are filtered out by the adsorbent to purify the chloride silane with an electronic grade silane. There is provided a silane chloride purification method.

In addition, according to another aspect of the present invention for achieving the above object, the step of performing the first purification by passing the silane chloride through a multi-stage distillation column; And passing the first purified chlorinated silane into the adsorption bed filled with the adsorbent for purifying the metal impurities, and in the process, the metal impurities contained in the chlorinated silane are caught by the adsorbent and filtered to purify the electronic grade with high purity. A silane chloride purification method is provided, comprising a second purification step of obtaining silane chloride.

The metal-based impurity purification adsorbent used in the silane chloride refining method is preferably made of spherical particles using a mixture containing 100 to 50% by weight of ocher powder and 0 to 50% by weight of microporous forming aid. The micro-pore forming aid includes at least one selected from the group consisting of kaolin, charcoal powder, and anion powder.

The chlorine silane refining method, in order to put the first purified chlorine silane into the adsorption bed in a gaseous state, by heating the primary purified chlorine silane in a liquid state above the boiling point to a gaseous state to the adsorption Feeding into a bed; And liquefying by condensing the secondary purified chloride silane in a gaseous state exiting the adsorption bed. In the case of supplying the first purified chlorinated silane to the adsorption bed in a gaseous state, it is preferable to supply from the upper side of the adsorption bed to be discharged downward.

The first purified chlorinated silane may be supplied to the adsorption bed in a liquid state. In this case, the first purified chlorine silane may be supplied from the lower side of the adsorption bed to be discharged upward.

On the other hand, according to another aspect of the present invention for achieving the above object, a silane chloride purification system having a multi-stage distillation column for the first purification of the chlorine silane to be purified, and a first storage tank for storing the first purified chlorinated silane The pump of claim 1, wherein the primary purified chlorine silane stored in the first storage tank is pressurized and sent to a suction bed through a pipe; And the metal impurities contained in the inside of the container are filled with adsorbent particles for removing metal-based impurities so that the first purified chlorinated silane enters one side of the container and exits to the other. There is provided a silane chloride purification system, characterized in that it has an adsorptive bed which is trapped in and filtered and discharges secondary chlorinated silane with high purity of electronic grade.

The adsorption bed is provided with a support plate and a cover plate, respectively, in the lower and upper portions of the vessel, and the adsorbent particles are filled in the space between the support plate and the cover plate, and the support plate and the cover plate are the primary purified chloride. Multiple openings are provided to allow passage of silane but not allow the adsorbent particles to escape.

The silane chloride purification system may further include a vaporizer disposed between the pump and the adsorption bed and configured to convert the primary purified chlorine silane in a liquid state to a boiling point or more and convert it into a gaseous state to be introduced into the adsorption bed. Can be.

The chlorine chloride purification system may further include a condenser for condensing and converting the gaseous secondary purified chlorine silane discharged from the adsorption bed into a liquid state.

According to another aspect of the present invention for achieving the above object, 100 to 50% by weight ocher powder; And it provides a silane chloride tablet adsorbent, characterized in that made of particles of a predetermined form using a mixture comprising 0 to 50% by weight of the microporous forming aid.

The micro-pore forming auxiliary agent preferably includes at least one selected from the group consisting of kaolin, charcoal powder, and anion powder.

It is preferable that the particle | grains of the said adsorbent are 0.1 mm or more and 8.0 mm or less.

The adsorbent particles are preferably sintered at a temperature between 500 ° C and 1,000 ° C.

The size of the ocher particles is preferably a fine size passed through a size equal to or smaller than 325 mesh (mesh).

According to the present invention, a boron trichloride (BCl ₃ ) and a boron-containing compound, a phosphorus trichloride (PCl ₃ ) and a phosphorus-containing compound contained in the silane chloride are removed using an adsorbent having an ocher component with a removal rate of 99% or more. It is possible to obtain a high purity electron trichloride silane of less than 1 ppb. The silane chloride purified at the removal rate of such metallic impurities may be used to prepare electronic grade silane chloride.

1 shows a schematic configuration of a silane chloride purification system according to the present invention.

(1) silane chloride purification system

1 shows the configuration of a system 10 for purifying silane chloride in two stages according to the present invention. The purification system 10 includes a multi-stage distillation column 12 for firstly purifying the chlorinated silane to be purified in order to remove boron-based and phosphorus-based compounds, which are metallic impurities contained in the silane chloride. The multi-stage distillation column 12 may use a conventionally known one. In the multi-stage distillation column 12, although metal impurities are removed, they may not be removed to an extent sufficient for the production of electronic grade silane chloride. For this reason, the purification system 10 according to the present invention further includes an adsorption bed 18 filled with the adsorbent 30 to purify the chloride silane firstly rectified in the multi-stage distillation column 12 once more. The adsorbent 30 contacts and removes the metallic impurities contained therein when the primary purified silane passes.

The suction bed 18 is, for example, a cylindrical container 18-1 having an open bottom and an upper part, and a support plate 18-2 and a cover plate 18-3 which respectively block the lower and upper parts of the container 18-1. And adsorbent particles 30 filled to fill the empty space between the support plate 18-2 and the cover plate 18-3. Each of the support plate 18-2 and the cover plate 18-3 is provided with a plurality of openings through which chlorinated silane, which is a purification target, can pass.

The pore size should be smaller than the diameter of the adsorbent particles 30 to allow passage of the first purified chlorinated silane but not allow the adsorbent particles 30 to escape. Such a configuration of the adsorption bed 18 is only one example, and any structure of the adsorption bed 18 is provided so long as the adsorbent particles 30 are accommodated therein so that the silane chloride to be purified can pass through the adsorbent particles 30. Does not matter.

For the second purification process of the silane chloride using the adsorption bed 18, a storage tank 14-1 for temporarily storing the first purified chlorine silane through the outlet of the multi-stage distillation column 12 will be provided. Can be. In addition, the purification system 10 also includes a pump 16 for introducing the primary purified chloride silane in the storage tank 14-1 into the adsorption bed 18 and passing it in contact with the adsorbent 30 filled therein. do. At the outlet of the adsorption bed 18, a storage tank 14-2 for storing secondary purified chlorinated silane is provided.

Further, the silane chloride to be purified may be supplied to the adsorption bed 18 in a gaseous state (to be described later). For this purpose, the chlorine chloride is heated between the pump 16 and the adsorption bed 18 to a boiling point or higher to vaporize it. It is necessary to arrange the vaporizer 17 to make. In addition, at the outlet side of the adsorption bed 18, a condenser 19 for cooling and liquefying the purified chlorinated silane in the gaseous state is provided.

(2) two-step purification process of silane chloride

The purified silane chloride is purified in two steps using the purification system 10 of FIG. 1. Primary purification is accomplished by passing silane chloride through a multi-stage distillation column 12 as is known in the art. Secondary purification is the purification of the first purified chlorinated silane through the adsorption bed 18 filled with the adsorbent 30. Specifically, the silane chloride purified first in the multi-stage distillation column 12 is stored in the storage tank 14-1, and then introduced into the adsorption bed 18 by the pump 16. The primary purified chlorosilane passes through the pores (pores) formed in each adsorbent particle while contacting the adsorbent particles packed therein while passing through the adsorbent bed 18. In the process, only the silane chloride purified by the high purity by filtering metal impurities such as boron trichloride (BCl ₃ ) and other boron compounds and phosphorus trichloride (PCl ₃ ) and phosphorus containing compounds contained in the silane chloride from the pores of the adsorbent The suction bed 18 exits.

The adsorbent to be filled in the adsorption bed 18 is made into particles of a predetermined size with the main component of ocher having excellent adsorptivity to metallic impurities. The inventors have learned from various experiments that the ocher component has a property of physically binding well with the metallic impurities contained in the silane chloride due to its self-adsorption capacity, and the conditions under which the adsorbent can be prepared to remove the metallic impurities. .

According to him, specifically, the ocher component adsorbent to be used for the secondary purification of silane chloride is preferably made by mixing the raw material of 100 to 50% by weight of the ocher powder and 0 to 50% by weight of the microporous forming aid. The micro-pore forming aid may be kaolin, charcoal powder or anionic powder. At least one of these kaolin, charcoal powder and anionic powder is mixed with the ocher powder to prepare the spherical ocher adsorbent, which helps to effectively form fine pores in the spherical ocher adsorbent. As the number of fine pores in the adsorbent increases, the adsorption performance of the metal impurity increases. If the ocher component is less than 50% by weight, the ability to remove the adsorbent is low, there is a problem that long-term use is difficult. In addition, there is a problem that the component change of the silane chloride may occur due to other components.

The main raw material ocher is not particularly limited, but it is preferable to use the ocher produced in Korea, the size of the ocher particles, for example, it is preferable to use the fine particles passed through the 325 mesh.

The adsorbent used for the adsorption bed 18 is prepared into particles of a predetermined form using the above raw material mixture. The form of the particles is preferably produced in a spherical shape advantageous in terms of ease of production and strength of the particles. However, of course, it is possible to produce other types of particles. The size of the spherical adsorbent particles containing ocher powder is preferably set in the range of about 0.1 mm or more and 8.0 mm or less in diameter. More preferably, the diameter of the adsorbent particles is 0.5 mm or more and 5.0 mm or less, and most preferably 0.8 mm or more and 3.0 mm or less. If the size of the adsorbent particles is 8.0mm or more, the void space becomes too large in the adsorbent filling rate, thereby reducing the purification efficiency of the metallic impurities. On the contrary, when the size of the adsorbent particles is 0.1 mm or less, the bed is almost filled with powder, so that the liquid or gaseous chloride silane exits out of the adsorption bed 18 together when passing through the adsorption bed 18. Problems may arise.

In addition, the prepared spherical particles are preferably subjected to a heat treatment at high temperature. This high temperature heat treatment can increase the bonding strength of the particles and can also remove the low volatile organic compounds contained in the particles. Although the heat processing temperature is not specifically limited, It is preferable to heat-process at 500 degreeC to 1000 degreeC high temperature.

The ocher spherical adsorbent thus prepared is excellent in absorbing capacity and has numerous fine pores (pores) therein. As the trichlorosilane passes through the micropores of the ocher-like spherical adsorbent 30 particles filling the inside of the adsorption bed 18, the metallic impurities contained in the trichlorosilane (that is, boron trichloride BCl ₃ And other boron compounds and PCl ₃ phosphorus trichloride And phosphorus containing compound component) are held in the adsorbent 30 by physical bonding with the micropores, while pure trichlorosilane passes through the micropores. Thereby, trichlorosilane purified by the electronic grade is obtained.

The silane chloride obtained through the primary rectification in the multistage distillation column 12 and stored in the storage tank 14-1 contains metallic impurities (boron boron trichloride BCl ₃₎ contained therein. And other boron compounds and PCl ₃ phosphorus trichloride And a phosphorus-containing compound) to pressurize the pump 16 and feed it to the adsorption bed 18. In supplying the silane chloride to the adsorption bed 18, the silane chloride may be supplied in the liquid phase, but in order to have a more effective removal efficiency, it is preferable to heat the boiling point above its boiling point and supply it in a gaseous state.

When supplied in the liquid phase, the silane chloride in the liquid phase comes into full contact with the adsorbent 30 filled therein while passing through the adsorption bed 18. Through such contact, metallic impurities contained in the chloride silane are trapped in the pores in the adsorbent, thereby preventing them from exiting the adsorption bed 18, and only pure chloride chloride passes through the adsorption bed 18 to the storage tank 14-2. Stored.

When the chloride silane is heated above the boiling point and supplied to the adsorption bed 18 in a gaseous state, the metallic impurities and the silane chloride are respectively in contact with the adsorbent 30 in the gaseous state. Therefore, there is an advantage that the metal-based impurities are more effectively adsorbed to the adsorbent 30. Since the boiling point of the silane chloride is about 40 ° C., the heating temperature for supplying the chloride silane in the gas state needs to be 40 ° C. or higher. In addition, heating to an excessively high temperature increases the pressure of the gas and increases energy consumption, but does not significantly affect the metal impurities removal effect. Experimental results show that the heating temperature of the silane chloride is preferably not higher than 120 ° C. More preferably, the silane chloride is heated in a temperature range of 50-100 ° C.

In addition, the direction in which the gaseous or liquid silane chloride is supplied to the adsorption bed 18 may be in any direction from the bottom to the top or vice versa. When the silane chloride is supplied in the liquid phase, supplying it from the bottom of the adsorption bed 18 to be discharged upward may contact the entire surface of the adsorbent 30 to effectively remove metal impurities. In the case of supplying the silane chloride to the adsorption bed 18 in a gaseous state, it is more effective to supply it from the upper side of the adsorption bed 18 to be discharged downward. Since the gas has an upward characteristic, supplying gas from the upward direction is effective in removing metal impurities by lengthening the contact time with the adsorbent by merging with the desired upward characteristic.

(3) Purification effect analysis

On the other hand, in order to determine the effect of the silane chloride purification method described above, the present inventors performed the component analysis of the silane chloride and metal impurities and the removal efficiency analysis of the metal impurities before and after passing through the adsorption bed 18 in the following manner: It was.

(3-1) Analysis of silane chloride component

Before and after passing the purified chlorinated silane through the adsorbent 30 in the adsorption bed 18, a predetermined amount of each sample was taken, and component analysis was performed on each sample by using gas chromatography. This is a task to find out what changes in the components of the silane chloride by purifying the chlorine silane to be passed through the adsorbent 30 of the adsorption bed (18).

(3-2) Analysis of Metal-based Impurity Removal Efficiency

The analysis of metal-based impurity removal efficiency was measured for boron and phosphorus in metal impurities by using an Inductively Coupled Plasma (ICP) method for the sample before and after passing through the adsorption bed 18. Using the equation below Purification efficiency was calculated.

Hereinafter, the effect of the present invention through the Examples and Comparative Examples according to the present invention.

Example 1

Prepare a standard solution of silane trichloride so that the content of boron trichloride and phosphorus trichloride is 100 ppb, store it in a storage tank 14-1, take a predetermined amount of sample, and conduct gas chromatography and inductively coupled plasma analysis. The components of the silane and the metallic impurities were analyzed. In the adsorption bed 18 is filled with a spherical adsorbent of ocher components made of the same components as shown in Table 1 and sintered at a temperature of 850 ° C. with a diameter of 20 mm and a height of 200 mm. The trichloride silane is supplied to the vaporizer 17 using the fixed quantity feed pump 16, and the heating temperature of the vaporizer 17 is set to 60 degreeC. The trichlorosilane heated to 60 ° C. to the adsorption bed 18 is supplied, and the purified trichlorosilane in the gaseous state passing through the adsorption bed 18 is cooled and liquefied in the condenser 19, and the storage tank 14-2. Are stored in. The predetermined amount of trichlorosilane obtained in this way was taken, and the content of trichlorosilane and metal impurities such as boron and phosphorus was analyzed using gas chromatography and inductively coupled plasma analysis. And the analysis results are shown in Table 2.

[Example 2]

Example 2 was tested and analyzed under the same conditions and methods as in Example 1, except that an adsorbent prepared with the components shown in Example 2 of Table 1 and a vaporizer temperature (80 ° C.) were applied. And the analysis results are shown in Table 2.

Example 3

Example 3 was tested and analyzed under the same conditions and methods as in Example 1, except that an adsorbent prepared with the components shown in Example 3 of Table 1 and a vaporizer temperature (70 ° C.) were applied. . And the analysis results are shown in Table 2.

Example 4

Example 4 was tested and analyzed under the same conditions and methods as in Example 1, except that an adsorbent prepared from the ingredients shown in Example 4 of Table 1 was used. And the analysis results are shown in Table 2.

Comparative Example 1

Comparative Example 1 was tested and analyzed under the same conditions and methods as in Example 1, except that an adsorbent prepared with the ingredients shown in Table 1 and a vaporizer temperature (70 ° C.) were applied. And the analysis results are shown in Table 2.

Comparative Example 2

Comparative Example 2 was tested and analyzed under the same conditions and methods as in Example 1, except that the adsorbent prepared with the components shown in Table 1 and the vaporizer temperature (70 ° C.) were applied. And the analysis results are shown in Table 2.

The results of the above embodiments and comparative examples are summarized in Table 2 below.

Example 1 Example 2 Example 3 Example 4 Comparative Example 1 Comparative Example 2 absorbent
ingredient
(wt%) ocher 100 80 80 80 40 30 Charcoal powder 20 60 40 Kaolin 20 30 Anion powder 20 Carburetor Temperature (℃) 60 80 70 60 70 80

Example 1 Example 2 Example 3 Example 4 Comparative Example 1 Comparative Example 2 % Before Passing Silane chloride 100 100 100 100 100 100 After passing
ingredient(%) Trichlorosilane 100 100 100 100 95 90 Other compounds 5 10 Before passing (A)
Metal (ppbw) Boron (B) 100 100 100 100 100 100 Phosphorus (P) 100 100 100 100 100 100 After passing (a)
Metal (ppbw) Boron (B) <0.5 <0.5 <0.5 <0.5 2.5 3.0 Phosphorus (P) <0.5 <0.5 <0.5 <0.5 5.0 10.0 Boron (B) removal rate (1-a / A X100,%) 99.5 ↑ 99.5 ↑ 99.5 ↑ 99.5 ↑ 97.5% 97% Phosphorus removal rate (1-a / A X100,%) 99.5 ↑ 99.5 ↑ 99.5 ↑ 99.5 ↑ 95% 90%

When the adsorbent containing more than 80% by weight of ocher was used, the removal rate of boron and phosphorus impurities was 99.5% or more. In contrast, when the adsorbents made using only about 30% by weight or about 40% by weight of ocher were used, it was confirmed that the impurity removal rates were lowered to about 97% and about 97.5%. These tests confirmed that the ocher component must be at least 50% by weight to achieve 99% or more impurity removal.

The present invention can be widely used to purify the silane chloride compound.

12: multi-stage distillation column 14-1, 14-2: storage tank
16: pump 17: carburetor
18: bed area 18-1: container
18-2: Support Plate 18-3: Cover Plate
19: condenser 30: adsorbent

Claims (19)

In the purification of silane chloride,
Chlorine silane was passed through an adsorption bed filled with adsorbent for sintering metal-based impurities, which was made into a particle form using a mixture containing 100 to 50% by weight of ocher powder and 0 to 50% by weight of microporous forming aids.
The method for purifying chlorine chloride, characterized in that the metal impurities contained in the chlorinated silane are filtered out by the adsorbent to purify the chlorinated silane with an electronic grade silane. The method of claim 1, wherein the microporous forming agent comprises at least one selected from the group consisting of kaolin, charcoal powder, anion powder. The method of claim 1, wherein the silane chloride is introduced into the adsorption bed in a liquid state or a gaseous state and passed through the adsorbent. The method of claim 1, wherein the particle size of the adsorbent is 0.1mm or more and 8.0mm or less. Primary purification of the silane chloride through a multi-stage distillation column; And
The first purified chlorine silane is introduced into the adsorption bed filled with the adsorbent for purifying metal impurities, and in the process, the metal impurities contained in the chlorinated silane are caught by the adsorbent and filtered and purified with high purity of electronic grade. A second purification step of obtaining silane chloride,
The adsorbent is a silane chloride purification method characterized in that the sintering was made in the form of particles using a mixture containing 100 to 50% by weight ocher powder and 0 to 50% by weight microporous forming aid. delete The method of claim 5, wherein the microporous forming agent comprises at least one selected from the group consisting of kaolin, charcoal powder, and anion powder. The method of claim 5, wherein the primary purified chlorine silane is introduced into the adsorption bed in a gaseous state, the liquid primary chlorinated silane is heated to a boiling point or more to a gaseous state to the adsorption bed Supplying; And condensing and liquefying the secondary purified chlorine silane in the gaseous state exiting the adsorptive bed. The method of claim 8, wherein when the primary purified chlorosilane is supplied to the adsorption bed in a gaseous state, the silane chloride purification method is supplied from an upper side of the adsorption bed to be discharged downward. The method of claim 5, wherein the first purified chlorinated silane is supplied to the adsorption bed in a liquid state, in which case the first purified chlorine silane is supplied from the bottom of the adsorption bed to be discharged upwards Silane chloride purification method. In the silane chloride purification system having a multi-stage distillation column for the first purification of the silane chloride to be purified, and a first storage tank for storing the first purified chlorosilane,
A pump for pressurizing the first purified chlorinated silane stored in the first storage tank and passing through the pipe to the following adsorption bed; And
The inside of the container is filled with an adsorbent for removing metal impurities, and the metal impurities contained therein are caught in the internal pores of the adsorbent while the primary purified chlorosilane enters one side of the container and exits to the other side. It is equipped with an adsorptive bed for filtering and discharging secondary purified chlorosilane with high purity of electronic grade,
The adsorbent is silane chloride purification system characterized in that the sintering was made in the form of particles using a mixture containing 100 to 50% by weight ocher powder and 0 to 50% by weight microporous forming aid. The method of claim 11, wherein the adsorption bed is provided with a support plate and a cover plate, respectively, in the lower and upper portions of the interior of the vessel, the adsorbent is filled in the space between the support plate and the cover plate, the support plate and the cover plate The silane chloride purification system, characterized in that a plurality of openings that allow the passage of the primary purified silane chloride, but the adsorbent does not escape. 12. The method of claim 11, further comprising a vaporizer disposed between the pump and the adsorptive bed, wherein the first purified chlorinated silane in a liquid state is heated to a boiling point or higher and converted into a gaseous state to be introduced into the adsorptive bed. Characterized in the silane chloride purification system. The chlorine silane purification system according to claim 13, further comprising a condenser for condensing and converting the secondary purified chloride silane in a gaseous state discharged from the adsorptive bed into a liquid state. Ocher powder 100 to 50% by weight;
Adsorption agent for silane chloride purification, characterized in that the mixture is sintered in the form of particles using a mixture containing 0 to 50% by weight of the microporous forming aid. 16. The chlorinated silane tablet adsorbent of claim 15, wherein the microporous forming aid comprises at least one selected from the group consisting of kaolin, charcoal powder, and anion powder. The silane chloride tablet adsorbent according to claim 15, wherein the particles of the adsorbent have a size of 0.1 mm or more and 8.0 mm or less. The adsorbent for silane chloride purification of claim 15, wherein the particles of the adsorbent are sintered at a temperature between 500 ° C and 1,000 ° C. The adsorbent for chlorine chloride refining of claim 15, wherein the ocher powder has a fine size passing through a size equal to or smaller than 325 mesh.

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