CN220283634U - Material comprehensive treatment system for polysilicon rectification process - Google Patents

Material comprehensive treatment system for polysilicon rectification process Download PDF

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CN220283634U
CN220283634U CN202321679343.6U CN202321679343U CN220283634U CN 220283634 U CN220283634 U CN 220283634U CN 202321679343 U CN202321679343 U CN 202321679343U CN 220283634 U CN220283634 U CN 220283634U
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raw material
trichlorosilane
tower
rectification
discharge port
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袁野
罗轩
涂彬
王波
冉进
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Sichuan Yongxiang Poly Silicon Co ltd
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Sichuan Yongxiang Poly Silicon Co ltd
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Abstract

The utility model discloses a material comprehensive treatment system for a polysilicon rectification process, which relates to the technical field of polysilicon and comprises a buffer storage tank and a rectification tower, wherein a discharge port of the buffer storage tank is connected with a material inlet of the rectification tower through a delivery pump, a discharge port at the bottom of the rectification tower is connected with a purification tower, a discharge port at the middle part of the rectification tower is connected with a trichlorosilane raw material storage tank, and a discharge port at the top of the rectification tower is connected with a disproportionation raw material tank. The system is used for rectifying the separation of the boron removal of the synthetic liquid and the cryogenic liquid and the slag slurry recovery liquid, not only can separate the trichlorosilane to increase the yield of a rectifying system, but also can reduce the introduction amount of boron and phosphorus elements in raw material rectification, and also can eliminate the problem that the trichlorosilane in the slag slurry recovery liquid circularly enters the cold hydrogenation system to inhibit the conversion rate of the trichlorosilane, thereby realizing the improvement of the yield of raw material rectification products and stable quality, and preparing the early stage for the improvement of the yield of the polysilicon in the future.

Description

Material comprehensive treatment system for polysilicon rectification process
Technical Field
The utility model relates to the technical field of polysilicon, in particular to a material comprehensive treatment system for a polysilicon rectification process.
Background
In the production link of Gao Chunjing silicon, the content of impurities such as boron trichloride, phosphorus trichloride, heavy metals and the like in the raw materials is ultrahigh, and the mass production and quality improvement of enterprises are greatly influenced. Under the condition, each high-purity crystal silicon enterprise seeks a new technical method, and partial boron trichloride and other impurities are expected to be removed by a pretreatment and post-refining method, so that the quality of raw materials is improved and stabilized, and the quality of Gao Chunjing silicon products is ensured.
The purpose of separation and purification is achieved by utilizing the difference of boiling points of substances in the traditional method for removing boron by rectification. The main operation is to control the temperature of the top and the bottom of the rectifying tower and the discharge amount of the bottom of the tower to remove the boron compound from the system. The method has high boron removal operation precision and cannot fluctuate on various control parameters.
The polysilicon slag slurry recovery product liquid is: the high-purity silicon tetrachloride which is discharged from the raw material rectifying device and contains substances such as heavy metals, high-boiling substances and the like is treated and purified by a slag slurry process, the high-purity silicon tetrachloride is recovered by the slag slurry recovery liquid, due to the slag discharge operation reason of a system, a small amount of trichlorosilane is contained in the slag slurry recovery liquid in the slag discharge process, the purified silicon tetrachloride contains the trichlorosilane and is sent to an original synthesized and rectified silicon tetrachloride purifying tower after being treated by the slag slurry recovery device, and then the low-boiling-point trichlorosilane and the purified silicon tetrachloride are sent back to cold hydrogenation, so that trichlorosilane circulation is formed, and the productivity is influenced.
The polysilicon cryogenic liquid is: tail gas generated in the production process of polycrystalline silicon is recycled after the chlorosilane (trichlorosilane, silicon tetrachloride and dichlorosilane) in the tail gas is condensed into liquid by utilizing a refrigerant when passing through a raw material rectification cryogenic device, a tail gas leaching cryogenic device and a tail gas recycling cryogenic device, the tail gas cryogenic liquid is sourced from three tail gas cryogenic devices, the cold materials of different devices are different, the three cryogenic liquids are intermittently fed to a raw material tank, and the components of the raw material tank are changed in height when the raw material tank receives the raw material, so that the separation operation of a synthetic rectifying tower is influenced.
Polycrystalline silicon synthesis liquid: the method is characterized in that the raw materials provided by the trichlorosilane synthesis process are used as the main components of the production raw materials from the trichlorosilane synthesis device, the trichlorosilane and the silicon tetrachloride are used as the main components, a small amount of dichlorosilane is used as the main components, the average boron content in the synthesis liquid is about 5000-10000 ppbw, and the ultra-high B is introduced into the original synthesis rectification treatment, so that the purification capacity is limited, the boron content of the refined trichlorosilane liquid is influenced, and the quality of Gao Chunjing silicon products is finally influenced.
Hydrogenation solution: the hydrogenated liquid (synthetic rectification raw material) comes from a cold hydrogenation device, contains more impurities, and is generally directly put into the synthetic rectification tower at the present stage, so that the feeding load and impurity removal load of the synthetic rectification tower are large, and the follow-up productivity planning is not facilitated.
The slag slurry, the cryogenic liquid, the synthetic liquid and the hydrogenated liquid at the present stage are generally directly put into a raw material rectifying system, and the B/P impurity content is too high and different from the content of various material components, so that the stability of the components in the raw materials is poor, and the workload of removing boron/phosphorus in raw material rectification and the difficulty of stable rectification control are directly increased; the boron/phosphorus content of the subsequent rectifying tower is increased, and the risk of exceeding the content of the boron/phosphorus of the refined trichlorosilane is caused; meanwhile, the cryogenic liquid and the synthetic liquid are directly put into an original rectification system, and are separated and purified by using a raw material rectification tower, so that the workload of the raw material rectification tower is increased, and the follow-up productivity improvement planning is not facilitated.
Accordingly, there is a need to provide a low cost, low energy-consuming material integrated processing system for polysilicon to solve the foregoing problems.
Disclosure of Invention
The utility model aims to provide a comprehensive material treatment system for a polysilicon rectification process, which is used for rectifying synthetic liquid, cryogenic liquid boron removal and slag slurry recovery liquid separation, can separate trichlorosilane to increase the yield of a rectification system, reduce the introduction amount of boron and phosphorus elements in raw material rectification, also solve the problem that the trichlorosilane in the slag slurry recovery liquid circularly enters a cold hydrogenation system to inhibit the conversion rate of the trichlorosilane, realize the improvement of the yield of raw material rectification products and stable quality, and provide early preparation for the improvement of the yield of polysilicon in the future.
In order to achieve the above purpose, the technical scheme adopted by the utility model is as follows:
the utility model provides a material integrated processing system of polycrystalline silicon rectification technology, includes cache storage tank and rectifying column, cache storage tank discharge gate links to each other with rectifying column material import through the delivery pump, purifying column is connected to the bottom of the tower discharge gate of rectifying column, and trichlorosilane raw materials storage tank is connected to the middle part discharge gate, and the anti-disproportionation feed tank is connected to the top of the tower discharge gate.
Four feed lines are connected to the feed inlet of the buffer storage tank, and are connected with a slag slurry pipeline of the slag slurry recovery device, a cryogenic liquid pipeline of the tail gas cryogenic device, a synthetic liquid pipeline of the trichlorosilane synthesis device and a hydrogenation liquid pipeline of the cold hydrogenation device, so that four raw materials of synthetic liquid, cryogenic liquid, slag slurry and hydrogenation liquid are respectively introduced.
The bottom discharge hole of the purification tower is connected with a cold hydrogenation slag slurry recovery processing device, the cold hydrogenation slag slurry recovery processing device is a plate type rectifying tower, and high-boiling substances and materials containing heavy metal impurities extracted from the bottom discharge hole of the purification tower are rectified and recovered.
The rectifying tower further comprises a feeding preheater, the feeding preheater is a double-channel winding tube type heat exchanger, the double channels of the feeding preheater are respectively connected with a discharging pipeline in the middle of the rectifying tower and a feeding pipeline of the rectifying tower, a material at the middle of high temperature is subjected to heat exchange with a material at relatively low temperature in the winding tube type heat exchanger, and the heated material is conveyed into a new rectifying tower.
The trichlorosilane raw material storage tank discharge port is connected with a raw material rectifying tower, and the trichlorosilane extracted from the middle discharge port in the raw material rectifying tower is separated, purified and utilized.
The top discharge port is connected with the anti-disproportionation raw material tank through an anti-disproportionation mixed solution feeding pipeline, and dichlorosilane extracted from the top of the tower is fully and uniformly mixed with silicon tetrachloride in the anti-disproportionation mixed solution feeding pipeline according to a certain proportion and then is introduced into the anti-disproportionation raw material tank for anti-disproportionation.
And a discharge hole of the anti-disproportionation raw material tank is connected with an anti-disproportionation device, and materials in the anti-disproportionation raw material tank are subjected to adsorption and reaction treatment to convert dichlorosilane into trichlorosilane.
The utility model has the beneficial effects that:
1. compared with the traditional rectification process, the utility model has the advantages that the upper, middle and lower adopted flow paths of the tower design not only meet the requirements of heavy removal, light removal and product recycling in the production process, but also greatly reduce the investment of equipment cost.
2. Aiming at the problem that trichlorosilane in the slag slurry recovery liquid circulates in the system, the trichlorosilane in the slag slurry recovery liquid is separated through the new tower, and the middle discharge port is fed into the raw material rectifying tower to be separated, purified and utilized, so that the cold hydrogenation conversion rate is improved, and the yield of refined trichlorosilane is increased.
3. The silicon tetrachloride containing high boron and phosphorus and high impurities is discharged from the novel tower kettle and sent to a purification tower, the silicon tetrachloride is recovered and utilized from the tower top, and the weight of the tower kettle is removed and then sent to a slag slurry recovery process for treatment; therefore, the problem of material pollution to a rectification system caused by introducing high-boron high-impurity chlorosilane outside the rectification of the raw material is solved, and the quality and stability of the refined trichlorosilane after the quantity is extracted by the rectification system are ensured.
4. When the high boron-phosphorus and high-impurity chlorosilane is treated, the whole quality of a production system is promoted to be improved, and the raw material rectifying tower has redundant purification capacity to match the synthesis and cold hydrogenation extraction capacity, so that the future capacity planning is satisfied.
5. The rectifying tower is used for researching the rectification process of removing boron from synthetic liquid and cryogenic liquid and separating slag slurry recovery liquid, not only can separate trichlorosilane to increase the yield of a rectification system, but also can reduce the introduction amount of boron and phosphorus elements in raw material rectification, and also can eliminate the problem that the trichlorosilane in the slag slurry recovery liquid circularly enters a cold hydrogenation system to inhibit the conversion rate of the trichlorosilane, thereby realizing the improvement of the yield of raw material rectification products and stable quality, and preparing the early stage for the improvement of the yield of polysilicon in the future.
Drawings
FIG. 1 is a schematic diagram of the structure of the present utility model;
FIG. 2 is a flow chart of the present utility model.
1, caching a storage tank; 2. a rectifying tower; 3. a transfer pump; 4. a feed line; 5. a purifying tower; 6. a trichlorosilane raw material storage tank; 7. a disproportionation raw material tank; 8. a feed preheater; 9. a cold hydrogenation slag slurry recovery treatment device; 10. a raw material rectifying tower; 11. a disproportionation mixed liquor feed line; 12. anti-disproportionation device
Detailed Description
The present utility model will be described in further detail with reference to examples, but embodiments of the present utility model are not limited thereto.
Example 1
The embodiment provides a material integrated processing system of polycrystalline silicon rectification technology, including buffer memory storage tank 1 and rectifying column 2, buffer memory storage tank discharge gate links to each other with rectifying column 2 material import through delivery pump 3, purifying column 5 is connected to rectifying column 2's bottom discharge gate, and trichlorosilane raw materials storage tank 6 is connected to the middle part discharge gate, and anti-disproportionation raw materials jar 7 is connected to the top of the tower discharge gate.
Four feed lines 4 are connected to the feed inlet of the buffer storage tank 1, and four raw materials including synthetic liquid, cryogenic liquid, slag slurry and hydrogenation liquid are respectively introduced into the four feed lines 4, wherein the four feed lines are connected with the slag slurry pipeline of the slag slurry recovery device, the cryogenic liquid pipeline of the tail gas cryogenic device, the synthetic liquid pipeline of the trichlorosilane synthesis device and the hydrogenation liquid pipeline of the cold hydrogenation device.
In the embodiment, the synthetic liquid, the slurry recovery liquid, the cryogenic liquid and the hydrogenated liquid are sent into a raw material storage tank 1 of a new rectifying tower, are uniformly mixed in the raw material storage tank 1, are then conveyed into the rectifying tower 1 for rectification through a conveying pump 3, the entered raw materials are heated by a steam reboiler, and then relatively low-boiling trichlorosilane and dichlorosilane are vaporized and rise to the top of the rectifying tower, and gas phase is condensed into liquid by a circulating water condenser at the top of the tower and flows into a reflux tank for storage; the liquid material which is pumped out of the reflux tank by the reflux pump is mostly returned to the rectifying tower to form a mass transfer and heat transfer process with the continuously rising gas phase, and finally, the purification circulation is continuously formed, and the material which contains little B/P and metal impurities is dichlorosilane and is conveyed to the anti-disproportionation raw material tank 7; the middle discharge hole is used for taking trichlorosilane as a material and conveying the trichlorosilane to a trichlorosilane raw material storage tank 6 through a tower kettle pump; and a material is silicon tetrachloride through a material outlet at the bottom of the tower and is conveyed into a purifying tower 5 for purification and refining. The slag slurry, the synthetic liquid, the cryogenic liquid and the hydrogenated liquid form a set of independent rectification device for removing boron and phosphorus impurities, thereby helping the quality and the production after pretreatment of a raw material rectification system; after the synthetic liquid is subjected to new rectification, separation and purification treatment, the final boron content is greatly reduced, the requirement of up-regulating the feed ratio after the technical improvement of the synthetic procedure is met, the feed ratio is improved, the yield of the refined trichlorosilane is increased, and the yield of the polysilicon is promoted to be improved. The synthetic liquid and the cryogenic liquid enter a new rectifying tower for treatment after raw material rectification treatment and technical optimization in the original flow, so that the raw material rectification is reduced; the hydrogenated liquid is split into a new rectifying tower for treatment, so that the raw material rectification is reduced in load, a reserved space is reserved for improving the yield, and the polysilicon yield is improved.
Example 2
Compared with the embodiment 1, the difference is that the rectifying tower 2 further comprises a feeding preheater 8, the feeding preheater 8 is a double-channel winding tube type heat exchanger, the double channels of the feeding preheater are respectively connected with a discharging pipeline in the middle of the rectifying tower and a feeding pipeline of the rectifying tower, and the rest structures are the same as those of the embodiment 1.
In the embodiment, trichlorosilane at the temperature of about 78 ℃ is obtained from the tower and is used for heating materials fed into the rectifying tower through a feeding heat exchanger; trichlorosilane taken out of the tower passes through a shell side of the heat exchanger, raw materials are subjected to heat exchange with trichlorosilane taken out of the tower through a tube side of the heat exchanger and then heated, and then enter a rectifying tower for separation and purification treatment; is beneficial to reducing the steam consumption of the rectifying tower, realizes the reduction of steam energy consumption and reduces the production cost investment.
Example 3
Compared with the embodiment 1, the embodiment is different in that a discharge hole at the bottom of the purifying tower 5 is connected with a cold hydrogenation slag slurry recycling device 9, and the cold hydrogenation slag slurry recycling device 9 is a plate type rectifying tower; a discharge hole of the trichlorosilane raw material storage tank 6 is connected with a raw material rectifying tower 10; the top discharge port is connected with the anti-disproportionation raw material tank 7 through an anti-disproportionation mixed solution feeding pipeline 11; the discharge port of the anti-disproportionation raw material tank 7 is connected with an anti-disproportionation device 12, and the rest of the structure is the same as that of the embodiment 1.
In the embodiment, dichlorosilane extracted from a discharge hole at the top of a rectifying tower and refined silicon tetrachloride are mixed in a feed line 11 of a disproportionation mixed solution according to silicon tetrachloride: after mixing the dichlorosilane in a ratio of 3.5:1, introducing the mixture into a disproportionation raw material tank 7 for disproportionation, adsorbing and reacting the material of the disproportionation raw material tank 7 by a disproportionation device 12, converting the dichlorosilane into trichlorosilane, feeding the trichlorosilane into raw material rectification to extract the trichlorosilane, and purifying the trichlorosilane into refined trichlorosilane; the trichlorosilane extracted from the discharge hole in the middle of the rectifying tower is sent to a trichlorosilane raw material storage tank 6 and then is led into a raw material rectifying tower 10 for rectifying and purifying to obtain refined trichlorosilane; the material silicon tetrachloride extracted from the discharge port at the bottom of the rectifying tower is introduced into a silicon tetrachloride purifying tower 5 for purification treatment, and then the material silicon tetrachloride is refined silicon tetrachloride, and high-boiling substances at the bottom of the purifying tower 5 and materials containing heavy metal impurities are connected with a cold-hydrogenation slag slurry recycling device 9 for recycling treatment; after new rectifying, separating and purifying treatment, the raw material flow slag liquid enters a cold hydrogenation process from the top of the raw material purifying tower in a recycling way, and after technical optimization, the raw material is rectified to produce refined trichlorosilane, so that the yield of the refined trichlorosilane is increased, and the yield of the polysilicon is promoted; the quality of the refined trichlorosilane product is stable, the contents of boron impurities, phosphorus impurities and total impurities are greatly reduced, and the quality stability and the improvement of the polysilicon product are promoted. Aiming at the problem that trichlorosilane in materials circulates in the system, the trichlorosilane in the slag slurry recovery liquid is separated through a new tower, and the middle part of the slag slurry recovery liquid is fed into raw material rectification, separation, purification and utilization, so that the improvement of cold hydrogenation conversion rate is facilitated, and meanwhile, the yield of refined trichlorosilane is increased.
It will be understood that the utility model has been described in terms of several embodiments, and that various changes and equivalents may be made to these features and embodiments by those skilled in the art without departing from the spirit and scope of the utility model. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the utility model without departing from the essential scope thereof. Therefore, it is intended that the utility model not be limited to the particular embodiment disclosed, but that the utility model will include all embodiments falling within the scope of the appended claims.

Claims (8)

1. A material comprehensive treatment system of a polysilicon rectification process is characterized in that: the device comprises a buffer storage tank (1) and a rectifying tower (2), wherein a discharge hole of the buffer storage tank (1) is connected with a feed hole of the rectifying tower (2) through a delivery pump (3), the feed hole is connected with four feed lines (4), and the four feed lines (4) are respectively connected with a slag slurry pipeline of a slag slurry recovery device, a cryogenic liquid pipeline of a tail gas cryogenic device, a synthetic liquid pipeline of a trichlorosilane synthetic device and a hydrogenation liquid pipeline of a cold hydrogenation device; the bottom discharge port of the rectifying tower (2) is connected with the purifying tower (5), the middle discharge port is connected with the trichlorosilane raw material storage tank (6), and the top discharge port is connected with the anti-disproportionation raw material tank (7).
2. The material integrated processing system according to claim 1, wherein: the rectifying tower further comprises a feeding preheater (8), and the feeding preheater (8) is a double-channel winding tube type heat exchanger.
3. The material integrated processing system according to claim 2, wherein: the double-flow channel of the feeding preheater (8) is respectively connected with a discharging pipeline in the middle of the rectifying tower and a feeding pipeline of the rectifying tower.
4. The material integrated processing system according to claim 1, wherein: the bottom discharge port of the purifying tower (5) is connected with a cold hydrogenated slag slurry recycling device (9).
5. The material integrated processing system according to claim 4, wherein: the cold hydrogenation slag slurry recycling device (9) is a plate type rectifying tower.
6. The material integrated processing system according to claim 1, wherein: the discharge port of the trichlorosilane raw material storage tank (6) is connected with a raw material rectifying tower (10).
7. The material integrated processing system according to claim 1, wherein: the top discharge port is connected with a disproportionation raw material tank (7) through a disproportionation mixed liquid feeding pipeline (11).
8. The material integrated processing system according to claim 7, wherein: and a discharge hole of the anti-disproportionation raw material tank (7) is connected with an anti-disproportionation device (12).
CN202321679343.6U 2023-06-29 2023-06-29 Material comprehensive treatment system for polysilicon rectification process Active CN220283634U (en)

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CN202321679343.6U CN220283634U (en) 2023-06-29 2023-06-29 Material comprehensive treatment system for polysilicon rectification process

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Application Number Priority Date Filing Date Title
CN202321679343.6U CN220283634U (en) 2023-06-29 2023-06-29 Material comprehensive treatment system for polysilicon rectification process

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