CN115040975A - Device for purifying silicon tetrachloride - Google Patents

Abstract

The invention discloses a device for purifying silicon tetrachloride. The front part of the chamber is the hydrolysis zone, and the latter part is the drying zone; the intake pipeline is connected to the front end of the hydrolysis zone, and the exhaust pipeline is connected to the rear end of the drying zone; the exhaust pipeline is connected to the monitoring system; The desiccant is crystalline hydrate, and the desiccant is evenly distributed in the drying area; the desiccant is silica gel or molecular sieve; the pipeline components, including the unqualified STC pipeline and the qualified STC pipeline, the qualified STC pipeline is connected with the monitoring system, and the unqualified STC pipeline is connected with the monitoring system. The two ends of the pipeline are respectively communicated with the monitoring system and the intake pipeline. The invention adopts the crystal water in the crystal hydrate to replace the liquid water to carry out the hydrolysis reaction, and realizes the safe and effective impurity removal for STC.

Description

A kind of device for purifying silicon tetrachloride

technical field

The invention relates to the technical field of polysilicon production, and more particularly, to a device for purifying silicon tetrachloride.

Background technique

The modified Siemens method is a preparation process for the production of polysilicon. polysilicon, this method produces a chlorosilane residue rich in trichlorosilane (TCS), silicon tetrachloride (STC) and dichlorodihydrosilicon (DSC). At present, there are two sources of TCS in the improved Siemens method. The first is to generate TCS by reacting hydrogen chloride with silicon powder, and the second is to use STC in the chlorosilane residue to prepare TCS by hydrogenation of STC and hydrogen. In the second method, the purity of the STC will affect the purity of the polycrystalline silicon raw material TCS, which in turn affects the quality of the polycrystalline silicon product. Therefore, the STC must be purified before preparing the TCS. The main impurity elements in STC are boron, phosphorus and various metal elements.

At present, the purification methods of STC are mainly rectification and partial hydrolysis. The rectification method uses distillation devices such as sieve tray towers, packed towers, and valve towers, and uses the difference in volatility between STC and various impurities to separate. Since the greater the polarity of the molecule, the greater the intermolecular force, the more energy required for the free movement of the molecule, and the higher its boiling point. Therefore, the rectification method has certain limitations for the removal of polar impurities, such as boron trichloride and phosphorus trichloride. The partial hydrolysis method is to use the characteristics of boron trichloride (BCl3) and other boron-containing complexes and chlorides of some elements such as iron and aluminum to be easily hydrolyzed, hydrated or complexed by water to form non-volatile compounds. miscellaneous.

Chinese patent CN103420381A relates to a method and device for recycling and disposing of silicon tetrachloride slurry in polysilicon production. The method adopted is a partial hydrolysis method. The hydrogen chloride gas generated by hydrolysis is absorbed and removed, and then neutralized with lye until the pH value is neutral, so as to produce a large amount of compound precipitates containing impurity elements, and the precipitates containing impurity elements are removed by solid-liquid separation. Generally speaking, this method can easily remove impurities that are hydrolyzed preferentially over silicon-hydrogen bonds and silicon-chlorine bonds. The generated orthosilicic acid is very easy to lose water and become silica gel after standing. Silica gel has a good adsorption effect on boron element, phosphorus trichloride and other polar impurities. But this patent needs to introduce a large amount of water into the hydrolysis device to carry out the hydrolysis reaction. When the chlorosilane carries out the hydrolysis reaction, the large amount of heat released by the hydrolysis reaction is very easy to cause the residual liquid water in the hydrolysis device to have phenomena such as bumping and volatilization. This in turn leads to an increase in the pressure in the hydrolysis device, and even an explosion of the hydrolysis device in severe cases. In order to reduce the possibility of explosion, the patent is equipped with a flow controller for monitoring the amount of water added. However, due to the uncontrollable heat released by hydrolysis, the patent still has certain potential safety hazards.

SUMMARY OF THE INVENTION

In view of the deficiencies in the prior art, the object of the present invention is to provide a device for purifying silicon tetrachloride, which realizes a safe and effective removal of STC by using the crystal water in the crystal hydrate to replace the liquid water for hydrolysis. miscellaneous.

In order to achieve the above object, the present invention provides the following technical solutions: a device for purifying silicon tetrachloride, which includes a purification device, a monitoring system and a pipeline assembly;

The purification device includes a shell with a long-shaped chamber inside, an air inlet pipeline and an air outlet pipeline; the front section of the elongated chamber is a hydrolysis area, and the rear section is a drying area; the air inlet pipeline is communicated with the front end of the hydrolysis area, and the outlet The gas pipeline is connected with the back end of the drying zone; the gas outlet pipeline is connected with the monitoring system; the adsorbent is evenly distributed in the hydrolysis zone, and the adsorbent is crystalline hydrate, and the drying zone is evenly distributed with a desiccant; the desiccant is silica gel or molecular sieve;

A pipeline assembly, which includes an unqualified STC pipeline and a qualified STC pipeline, the qualified STC pipeline is connected with the monitoring system, and the two ends of the unqualified STC pipeline are respectively connected with the monitoring system and the intake pipeline.

By adopting the above-mentioned technical scheme, the present invention can make the STC uniformly contact with the crystal water in the process of passing through the hydrolysis zone, so that the impurities in the STC can be fully reacted with the crystal water, and the impurity removal effect is improved; The STC in the drying zone will fully remove the water in the drying zone, reducing the residual water content in the elongated chamber, thereby reducing the possibility of bumping and evaporation in the purification device, and then explosion. Moreover, because the present invention uses the crystal water in the crystal hydrate to replace the liquid water to carry out the hydrolysis reaction, and utilizes the dehydration of the crystal hydrate to absorb the heat generated by the hydrolysis reaction, further reducing the explosion of the hydrolysis device due to excessive temperature and excessive air pressure. possibility.

The present invention further provides that: the crystal hydrate is acetamide containing crystal water, or sodium alginate containing crystal water, or cellulose containing crystal water.

By adopting the above technical scheme, the present invention utilizes the characteristics of the above three substances as organic complexing agents to adsorb metal element impurities in the STC, and the above three substances have larger molecules, higher boiling points, and stable properties, which are difficult to With the STC gas leaving the purification unit, the possibility of introducing new impurities is reduced.

The present invention is further provided that: the purification device further comprises an adsorbent carrier, the adsorbent carrier is evenly distributed on the adsorbent carrier, and the adsorbent carrier is evenly distributed in the hydrolysis zone; the adsorbent carrier is silica gel or modified resin.

By adopting the above technical scheme, when the STC passes through the silica gel, the water molecules and other polar impurities therein can be adsorbed and removed by the silica gel. When STC passes through the modified resin, the modified resin can adsorb the water molecules in it and complex the polar impurity elements in it.

The present invention is further provided as follows: the purification device further comprises a plurality of first gas path guide plates fixed in the hydrolysis zone, the plurality of first gas path guide plates are linearly arranged along the length direction of the hydrolysis zone, and the hydrolysis zone is spaced into a plurality of zones, One side of each first air path guide plate is provided with a ventilation port, the ventilation ports of two adjacent first air path guide boards are mutually displaced, and each two adjacent first air path guide boards are evenly filled with adsorbent carriers.

By adopting the above technical solution, the arrangement of the first gas path guide plate increases the path of the STC in the hydrolysis zone, increases the residence time of the STC in the hydrolysis zone, and makes the hydrolysis reaction more uniform and sufficient.

The present invention further provides that: the purification device further comprises a first porous baffle fixed at the end of the drying zone, and the desiccant is uniformly filled between the hydrolysis zone and the first porous baffle.

By adopting the above technical solution, the arrangement of the first porous baffle can reduce the possibility of the silica gel entering the gas outlet pipeline with the STC and leaving the elongated chamber without preventing the STC from entering the gas outlet pipeline.

The present invention further provides that: the purification device further comprises two second porous baffles fixed at both ends of the desiccant, and the desiccant is uniformly filled between the two second porous baffles.

The present invention is further provided as follows: the purification device further comprises a plurality of adsorption boxes fixed in the elongated chamber, the front end of each adsorption box is located at the front end of the hydrolysis zone, and the rear end is located at the rear end of the drying zone; each adsorption box is a strip The part of each adsorption box in the hydrolysis zone is filled with adsorbent carrier, and the part in the drying zone is filled with desiccant; all the adsorption boxes are parallel to the length direction of the elongated chamber, and are kept between each other. There are gaps.

The present invention is further provided as follows: the purification device further includes a second gas path guide plate, a plurality of adsorption boxes divide the space in the elongated chamber into a plurality of linearly arranged channels, and one end of each channel is blocked by a second gas path guide plate. Two gas path guide plates, two gas path guide plates corresponding to two adjacent channels are respectively located in the hydrolysis zone and the drying zone.

By adopting the above technical solution, the arrangement of the second gas path guide plate enables the STC to be in uniform contact with the adsorbent and the desiccant before entering the gas outlet pipeline.

The present invention is further arranged as follows: it also includes two air circuit control valves, one air circuit control valve controls the opening and closing of the air circuit between the monitoring system and the unqualified STC pipeline, and the other air circuit control valve controls the monitoring system to output the qualified STC pipeline. Air circuit on and off.

By adopting the above technical solution, the setting of the gas circuit control valve is convenient for the operator to interrupt the gas circuit for maintenance when problems occur in the gas circuit of the qualified STC or the unqualified STC gas circuit of the monitoring system.

The present invention is further provided as follows: it further comprises a purification device for purifying the output STC of the gas outlet pipeline, and the purification device is communicated with the monitoring system.

By adopting the above technical scheme, the present invention further separates and removes the metal impurities in the STC through the purification device.

To sum up, the present invention has the following beneficial effects compared to the prior art:

1. The present invention can make the STC uniformly contact with the crystal water in the process of passing through the hydrolysis zone, so that the impurities in the STC can be fully reacted with the crystal water, and the impurity removal effect is improved.

2. The present invention fully removes the moisture in the drying zone through the STC in the hydrolysis zone, reduces the residual water content in the elongated chamber, reduces the heat released by the purification device due to hydrolysis, and causes the residual water to boil and evaporate. Possibility , thereby reducing the possibility of explosion of the purification device.

3. The present invention uses the crystal water in the crystal hydrate to replace the liquid water to carry out the hydrolysis reaction, and uses the dehydration of the crystal hydrate to absorb the heat generated by the hydrolysis reaction, further reducing the explosion of the hydrolysis device due to excessive temperature and excessive air pressure. possibility.

Description of drawings

1 is a schematic diagram of the basic structure of Embodiment 1 of the present invention;

Fig. 2 is the full cross-sectional view of the purification device in Example 1 of the present invention;

3 is a full cross-sectional view of the purification device in Example 2 of the present invention;

FIG. 4 is a full cross-sectional view of the purification device in Example 3 of the present invention.

In the figure: 1. Purification device; 11. Housing; 111. Elongated chamber; 12. Inlet pipeline; 13. Outlet pipeline; 14. First gas path guide plate; Hole baffle; 16. Second porous baffle plate; 17. Adsorption box; 18. Second gas path guide plate; 2. Monitoring system; 3. Purification device; 5. Adsorbent carrier; 6. Desiccant; 7. Qualified STC pipeline; 8. Unqualified STC pipeline.

Detailed ways

The technical solutions of the present invention will be clearly described below with reference to the accompanying drawings. Obviously, the described embodiments are not all embodiments of the present invention, and all other The embodiments all belong to the protection scope of the present invention.

It should be noted that the terms "center", "upper", "lower", "horizontal", "left", "right", "front", "rear", "horizontal", "vertical", etc. indicate the orientation or The positional relationship is based on the orientation or positional relationship shown in the accompanying drawings, which is only for the convenience of describing the present invention and simplifying the description, and does not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, Therefore, it should not be construed as a limitation of the present invention.

Example 1

As shown in Figure 1-2, it is a schematic diagram of Example 1 of the present invention, a device for purifying silicon tetrachloride, which includes a purification device 1, a monitoring system 2 for detecting whether the impurity content in the STC is qualified, and pipeline components; purification; Device 1, which includes a casing 11 with a long chamber 111 inside, an inlet pipe 12 and an outlet pipe 13 for conveying STC; The road 13 is communicated; the gas outlet pipeline 13 is also communicated with the monitoring system 2, so that the purified STC is sent to the monitoring system 2; There is an adsorbent, and a desiccant 6 is evenly distributed in the drying area; the adsorbent is a crystalline hydrate, and the desiccant 6 is a granular silica gel capable of adsorbing polar molecules. The pipeline assembly, which includes the unqualified STC pipeline 8 and the qualified STC pipeline 7, the qualified STC pipeline 7 is connected with the monitoring system 2 to output the STC with qualified impurity content; the two ends of the unqualified STC pipeline 8 are connected to the monitoring system The system 2 is communicated with the intake line 12 , so that the STC with unqualified impurity content can be re-sent into the elongated chamber 111 through the intake line 12 .

When the STC enters the hydrolysis zone from the intake line 12, since the STC is in a gaseous state and the temperature is relatively high, when it contacts with the crystal hydrate, the crystal hydrate is easily dehydrated, so that the crystal water easily interacts with the trichloride in the STC. Impurities such as boron undergo a hydrolysis reaction to generate non-volatile compounds; taking the hydrolysis of boron trichloride as an example, the reaction mechanism is: BCl ₃ +3H ₂ O=B(OH) ₃ +3HCl. Moreover, crystal water can also be complexed with impurities such as boron trichloride in STC to form non-volatile complexes, such as B(OH) ₃ ; in addition, a small part of STC and crystal water can be hydrolyzed to form orthosilicic acid (H ₂ SiO ₄ ), the reaction formula is: SiCl ₄ +4H ₂ O=H ₂ SiO4+4HCl, with the help of the property of orthosilicic acid to easily lose water and become silica gel, silica gel is generated to help adsorb water molecules and polar impurities. Subsequently, the STC in the hydrolysis zone enters the drying zone, and the water molecules and polar impurities in the STC are further adsorbed and removed by silica gel. Subsequently, the STC leaving the drying zone will leave the purification device 1 through the gas outlet pipeline 13, and enter the monitoring system 2 to detect the impurity content, so as to output the STC with qualified impurity content.

The process of crystal hydrate losing crystal water is the breaking of chemical bonds, which needs to absorb heat. In the present embodiment, the STC will be uniformly contacted with the crystal water in the process of passing through the hydrolysis zone, so that the impurities in the STC can fully react with the crystal water, thereby improving the impurity removal effect; at the same time, the STC passing through the hydrolysis zone will be in The moisture in the drying zone is fully removed, the residual water content in the elongated chamber 111 is reduced, and the heat released by the purification device 1 due to hydrolysis is reduced, resulting in the possibility of the residual water bumping and evaporating, thereby reducing the explosion of the purification device 1. possibility. In addition, in this embodiment, the crystalline water in the crystalline hydrate is used instead of liquid water for the hydrolysis reaction, and the dehydration of the crystalline hydrate is used to absorb the heat generated by the hydrolysis reaction, which further reduces the explosion of the hydrolysis device due to excessively high temperature and excessive air pressure. possibility.

Specifically, the elongated chamber 111 in this embodiment is in the shape of a capsule, and the two ends of the chamber 111 are smoothly contracted toward the air inlet pipe 12 and the air outlet pipe 13 respectively, so that the STC can smoothly enter the hydrolysis zone and smoothly leave the elongated chamber. Room 111.

specific. In this embodiment, the diameter of the intake pipe 12 is larger than that of the exhaust pipe 13, so that the flow rate of the exhaust pipe 13 is smaller than the flow rate of the intake pipe 12, so as to increase the residence time of the STC in the elongated chamber 111, and to facilitate the STC In the elongated chamber 111, it is fully contacted with crystal water and silica gel.

Specifically, the purification device 1 further includes an adsorbent carrier 5, the adsorbent is evenly distributed on the adsorbent carrier 5, and the adsorbent carrier 5 is evenly distributed in the hydrolysis zone; the adsorbent carrier 5 is silica gel, and the carrier can be filled in the adsorption column or In a functional container similar to an adsorption column.

Specifically, the purification device 1 further includes a plurality of first gas path guide plates 14 located in the hydrolysis zone and fixedly connected to the inner side wall of the housing 11 . In multiple areas, one side of each first air path guide plate 14 is provided with a ventilation port 141 that facilitates the passage of STC, and the ventilation ports 141 of two adjacent first air path guide plates 14 are misaligned with each other. The adsorbent carrier 5 is uniformly filled in an air passage guide plate 14 . The arrangement of the first gas path guide plate 14 allows the STC to pass through the hydrolysis zone only through the vent 141, which increases the path of the STC in the hydrolysis zone, increases the residence time of the STC in the hydrolysis zone, and makes the hydrolysis reaction more uniform and sufficient.

Specifically, in this embodiment, the first air path guide plates 14 are divided into two groups, the two groups of the first air path guide plates 14 are arranged at intervals, and the ventilation openings 141 of the first air path guide plates 14 are located at the top of the elongated chamber 111 . The ventilation openings 141 of the other group of the first gas path guide plates 14 are located at the bottom of the elongated chamber 111 to further increase the path of the STC in the hydrolysis zone.

Specifically, the purification device 1 further includes a first porous baffle 15 located at the end of the drying zone and fixedly connected to the inner wall of the casing 11 , and the desiccant 6 is uniformly filled between the hydrolysis zone and the first porous baffle 15 . The arrangement of the first porous baffle 15 can reduce the possibility of the silica gel entering the gas outlet pipe 13 along with the STC and leaving the elongated chamber 111 without preventing the STC from entering the gas outlet pipe 13 .

This embodiment also includes two gas circuit control valves, one gas circuit control valve controls the on-off of the gas circuit between the monitoring system 2 and the unqualified STC pipeline, and the other gas circuit control valve controls the monitoring system 2 and the qualified STC pipeline The gas path between 7 is on and off. The setting of the gas path control valve is convenient for the operator to control the on-off of the gas path between the monitoring system 2 and the qualified STC pipeline 7 or the unqualified STC pipeline 8 for maintenance.

This embodiment also includes a purification device 3 for purifying the STC output from the gas outlet pipeline 13. The gas outlet pipeline 13 is communicated with the purification device 3, and the purification device 3 further separates and removes impurities in the STC. The STC purified by the purification device 3 will be sent to the monitoring system 2 for impurity content assessment.

Specifically, in this embodiment, the purification device 3 is a device that uses rectification to remove impurities in the STC, so as to further remove the metal element impurities therein, and for a very small amount of macromolecular substances such as acetamide mixed in the STC and HCl, which can also be removed by rectification.

Specifically, the monitoring system 2 in this embodiment uses infrared spectroscopy to detect impurities in the STC.

In this example, the crystal hydrate is acetamide containing crystal water. As an organic complexing agent, acetamide can adsorb metal element impurities in STC. Its molecule is large, its boiling point is high, and its properties are stable. It is difficult to leave the purification device with the STC gas, reducing the possibility of introducing new impurities. Moreover, due to the heat brought by the gaseous STC and the heat generated by the hydrolysis reaction in the hydrolysis zone, the temperature is relatively high, so that the acetamide (CH3CONH2) has a certain probability of being dehydrated to form acetonitrile (CH3CN), and acetonitrile also has metal element impurities. Good complexation can remove metal element impurities in STC. Because the boiling point of acetonitrile is also higher than that of STC, and its properties are relatively stable, it is difficult to leave the purification device with the STC gas, and it is not easy to introduce new impurities.

The ratio of acetamide crystal water adsorbent and silica gel desiccant is 10:1 to 1:1, and the optimal ratio is 4:1. The impurity content in the STC and original STC obtained after purification is shown in Table 1:

Table 1 corresponds to STC impurity content

Impurities (units) original content final content P(ppba) 0.68 0.09 B(ppba) 0.58 0.02 Fe(pptw, 10-9) 3 0.39 Cr(pptw, 10-9) 2 0.23 Zn(pptw, 10-9) 1 0.14

To sum up, the present embodiment can make STC uniformly contact with the crystal water therein in the process of passing through the hydrolysis zone, so that the impurities in the STC can be fully reacted with the crystal water, and the impurity removal effect is improved; Simultaneously by hydrolysis The STC in the drying zone will fully remove the moisture in the drying zone, reducing the residual water content in the elongated chamber 111, reducing the heat released by the purification device 1 due to hydrolysis, resulting in the possibility of residual water bumping and evaporation, thereby reducing the Possibility of explosion of purification unit 1. In addition, in this embodiment, the crystalline water in the crystalline hydrate is used instead of liquid water for the hydrolysis reaction, and the dehydration of the crystalline hydrate is used to absorb the heat generated by the hydrolysis reaction, which further reduces the explosion of the hydrolysis device due to excessively high temperature and excessive air pressure. possibility.

Example 2

As shown in FIG. 3 , it is a full cross-sectional view of the purification device 1 in Example 2 of the present invention. The difference between this embodiment and embodiment 1 is as follows:

In this embodiment, the adsorbent carrier 5 is a weakly basic modified resin with a bulk density of 0.40-0.60/ml. The modified resin can adsorb water molecules in STC and complex polar impurity elements. The desiccant 6 is molecular sieve, which is a synthetic hydrated aluminosilicate or natural zeolite with the function of screening molecules. The crystal cavity of molecular sieve has strong polarity, which enables molecular sieve to generate strong adsorption force for molecules containing polar groups.

In this embodiment, the purification device 1 further includes two second porous baffles 16, which are respectively located at both ends of the drying zone and are fixedly connected to the inner wall of the casing 11, and the molecular sieves are evenly filled in the two porous baffles 16. between the baffles. Since there are many water molecules in the hydrolysis zone, the two second porous baffles 16 and the inner wall of the casing 11 form an isolation space, which can isolate the water molecules in the hydrolysis zone as far as possible outside the drying zone, and improve the drying effect of the desiccant 6 . In this embodiment, a gap is left between the hydrolysis zone and the drying zone, so as to further separate the hydrolysis zone and the drying zone, and reduce the possibility of water molecules in the hydrolysis zone entering the drying zone.

In this embodiment, there is no purification device 3 , and the gas outlet pipeline 13 is directly connected to the monitoring system 2 .

The impurity content in the STC and the original STC obtained by the purification of the present embodiment is shown in Table 2, and the impurity content in the STC is effectively reduced after passing through the purification device;

Table 2 corresponds to STC impurity content

Impurities (units) original content final content P(ppba) 0.68 0.08 B(ppba) 0.58 0.03 Fe(pptw, 10-9) 3 0.32 Cr(pptw, 10-9) 2 0.20 Zn(pptw, 10-9) 1 0.22

Example 3

As shown in FIG. 4 , it is a full cross-sectional view of the purification device 1 in Example 3 of the present invention. The difference between this embodiment and embodiment 2 is as follows:

Specifically, the purification device 1 also includes a plurality of adsorption boxes 17 that are fixedly connected to the inner side wall of the housing 11. The front end of each adsorption box 17 is located at the front end of the hydrolysis zone, and the rear end is located at the rear end of the drying zone; each adsorption box 17 is a bar-shaped , and the box body is evenly opened with a plurality of holes; the part of each adsorption box 17 in the hydrolysis zone is filled with the adsorbent carrier 5, and the part in the drying zone is filled with molecular sieve; all the adsorption boxes 17 are parallel to the length direction of the elongated chamber 111, and leave a gap between them. In this embodiment, four suction boxes 17 are provided.

Specifically, the purification device 1 further includes a second gas path guide plate 18; the four adsorption boxes 17 divide the elongated chamber 111 into five linearly arranged channels, all of which are connected to the air inlet pipeline 12 and the air outlet pipeline 13; One end of each channel is blocked with a second gas path guide plate 18, and the two gas path guide plates corresponding to two adjacent channels are located at the front end of the hydrolysis zone and the rear end of the drying zone, respectively. The setting of the second air path guide plate 18 allows the STC to enter the air outlet pipeline 13 only through the adsorption box 17, and because the path of the STC after passing through an adsorption box 17 is not a straight line along the length of the channel, this makes the STC very difficult It is possible to come into contact with another adsorption box 17 on the side wall of the channel, or even pass through another adsorption box 17, so that the STC can be in sufficient contact with the adsorbent and desiccant 6 for the hydrolysis reaction and the removal of excess water.

The impurity content in the STC and the original STC obtained by the purification of the present embodiment is shown in Table 3, and the impurity content in the STC is effectively reduced after passing through the purification device;

Table 3 corresponds to STC impurity content

Impurities (units) original content final content P(ppba) 0.68 0.13 B(ppba) 0.58 0.05 Fe(pptw, 10-9) 3 0.42 Cr(pptw, 10-9) 2 0.10 Zn(pptw, 10-9) 1 0.12

The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims (10)

1. a device for purifying silicon tetrachloride, characterized in that: comprising a purification device (1), a monitoring system (2) and a pipeline assembly; A purification device (1), comprising a casing (11) with a long-shaped chamber (111) opened therein, an air inlet pipeline (12) and an air outlet pipeline (13); the front section of the long-shaped chamber (111) is a hydrolysis zone , the rear section is the drying area; the air inlet pipeline (12) is communicated with the front end of the hydrolysis zone, and the air outlet pipeline (13) is communicated with the rear end of the drying zone; the air outlet pipeline (13) is communicated with the monitoring system (2); An adsorbent is distributed, and the adsorbent is a crystalline hydrate; a desiccant (6) is evenly distributed in the drying area, and the desiccant (6) is silica gel or molecular sieve; A pipeline assembly, comprising an unqualified STC pipeline (8) and a qualified STC pipeline (7), the qualified STC pipeline (7) is communicated with the monitoring system (2), and the two ends of the unqualified STC pipeline (8) are respectively It communicates with the monitoring system (2) and the intake line (12). 2. A device for purifying silicon tetrachloride according to claim 1, wherein the crystal hydrate is the acetamide containing crystal water, or the sodium alginate containing crystal water, or the crystal water containing cellulose. 3. A device for purifying silicon tetrachloride according to claim 1, characterized in that: the purification device (1) further comprises an adsorbent carrier (5), and the adsorbent is evenly distributed between the baffles for adsorption On the agent carrier (5), the adsorbent carrier (5) is evenly distributed in the hydrolysis zone; the adsorbent carrier (5) can be silica gel or modified resin, and the carrier can be filled in an adsorption column or a functional container similar to an adsorption column. 4. A device for purifying silicon tetrachloride according to claim 3, wherein the purification device (1) further comprises a plurality of first gas path guide plates (14) fixed in the hydrolysis zone, and a plurality of The first gas path guide plates (14) are linearly arranged along the length direction of the hydrolysis zone, each first gas path guide plate (14) is provided with a vent (141) on one side, and two adjacent first gas path guide plates (14) ) of the ventilation openings (141) are displaced from each other, and the adsorbent carriers (5) are evenly filled in every two adjacent first gas path guide plates (14). 5. A device for purifying silicon tetrachloride according to claim 4, characterized in that: the purification device (1) further comprises a first porous baffle plate (15) fixed at the end of the drying zone, the desiccant (6) It is uniformly filled between the hydrolysis zone and the first porous baffle (15). 6. A device for purifying silicon tetrachloride according to claim 4, wherein the purifying device (1) further comprises two second porous baffles fixed at both ends of the desiccant (6) respectively (16), the desiccant (6) is uniformly filled between the two second porous baffle plates (16). 7. A device for purifying silicon tetrachloride according to claim 3, wherein the purification device (1) further comprises a plurality of adsorption boxes (17) fixed in the elongated chamber (111). ), the front end of each adsorption box (17) is positioned at the front end of the hydrolysis zone, and the rear end is positioned at the rear end of the drying zone; each adsorption box (17) is a strip and all opens a plurality of holes; each adsorption box (17) is positioned at the hydrolysis zone Part of the zone is filled with adsorbent carrier (5), and part of the drying zone is filled with desiccant (6); all adsorption boxes (17) are parallel to the length direction of the elongated chamber (111), and there are gaps between them . 8. A device for purifying silicon tetrachloride according to claim 7, characterized in that: the purification device (1) further comprises a second gas path guide plate (18), and a plurality of adsorption boxes (17) will be long The space in the bar-shaped chamber (111) is divided into a plurality of linearly arranged channels, one end of each channel is blocked with a second air path guide plate (18), and two air path guide plates corresponding to two adjacent channels They are located in the hydrolysis zone and the drying zone, respectively. 9. a kind of device of purifying silicon tetrachloride according to claim 1, is characterized in that: also comprise two gas circuit control valves, a gas circuit control valve control monitoring system (2) and substandard STC pipeline between The on-off of the gas path between the two, another gas path control valve controls the monitoring system (2) to output the on-off of the gas path of the qualified STC. 10. a kind of device for purifying silicon tetrachloride according to claim 1, is characterized in that: also comprises the purification device (3) that the output STC of the gas outlet pipeline (13) is purified, the purification device (3) and monitoring System (2) is connected.

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