CN115092934A - Method and system for controlling content of dichlorosilane in refined trichlorosilane - Google Patents

Method and system for controlling content of dichlorosilane in refined trichlorosilane Download PDF

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Publication number
CN115092934A
CN115092934A CN202210702339.0A CN202210702339A CN115092934A CN 115092934 A CN115092934 A CN 115092934A CN 202210702339 A CN202210702339 A CN 202210702339A CN 115092934 A CN115092934 A CN 115092934A
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dichlorosilane
trichlorosilane
separation tower
tower
pipeline
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彭中
李寿琴
杨强
杜炳胜
汪云清
杨成
刘阳
王世棋
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Yunnan Tongwei High Purity Crystalline Silicon Co ltd
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Yunnan Tongwei High Purity Crystalline Silicon Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/08Compounds containing halogen
    • C01B33/107Halogenated silanes
    • C01B33/1071Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P90/00Enabling technologies with a potential contribution to greenhouse gas [GHG] emissions mitigation
    • Y02P90/02Total factory control, e.g. smart factories, flexible manufacturing systems [FMS] or integrated manufacturing systems [IMS]

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Abstract

The invention discloses a method for controlling the content of dichlorosilane in refined trichlorosilane, which belongs to the technical field of polycrystalline silicon production and comprises the following steps: the method comprises the steps of feeding synthesized high-purity trichlorosilane and recovered trichlorosilane into a separation tower for mixing, heating the separation tower, vaporizing chlorosilane, condensing dichlorosilane to be in a liquid state through a condenser, extracting part of dichlorosilane, feeding the rest part of dichlorosilane back to the separation tower to serve as reflux liquid, obtaining a pressure value and a temperature value in a tower kettle of the separation tower, judging the relation between the content of the dichlorosilane in the separation tower and the pressure value and the temperature value of the separation tower through a DCS (distributed control System) system, and determining the extraction amount of the dichlorosilane.

Description

Method and system for controlling content of dichlorosilane in refined trichlorosilane
Technical Field
The invention relates to the technical field of polysilicon production, in particular to a method and a system for controlling the content of dichlorosilane in refined trichlorosilane.
Background
In the production of polycrystalline silicon, the content of dichlorosilane needs to be controlled in the refining of trichlorosilane used by the reduction furnace, and the content of dichlorosilane is usually controlled to be 2-5%. With the continuous improvement of the deposition rate and product quality requirements of various enterprises in the reduction process, the content of dichlorosilane in the refined trichlorosilane for reduction needs to be controlled in a very narrow range.
The method for controlling the content of dichlorosilane in refined trichlorosilane in the industry at present mainly controls the content of dichlorosilane in the recovered refined trichlorosilane by controlling the yield of dichlorosilane at the tower top of a separation tower for recovering and rectifying dichlorosilane, and then mixes the recovered refined trichlorosilane with the synthesized and rectified trichlorosilane in a refined trichlorosilane buffer tank to reach the required concentration. The method is an empirical method, and the extraction amount at the top of the dichlorosilane separation tower is estimated mainly according to the content of dichlorosilane in the recovered and rectified raw materials, so that the concentration of dichlorosilane in the refined trichlorosilane is controlled.
In the method, when the concentration fluctuation of dichlorosilane in the raw material is large, the problem of large concentration fluctuation of dichlorosilane in the refined trichlorosilane exists; in addition, the final product of refined trichlorosilane is the mixture of recovered refined trichlorosilane and synthetic rectified refined trichlorosilane, and the flow rates of two materials generally fluctuate to a certain extent, so that the concentration of dichlorosilane in the final refined trichlorosilane fluctuates, and the product quality is unstable.
Disclosure of Invention
The invention aims to provide a method and a system for controlling the content of dichlorosilane in the refined trichlorosilane, which solve the problem that the product quality is unstable due to large fluctuation of the ratio of trichlorosilane to dichlorosilane in the process of inputting raw materials to refine trichlorosilane in the reduction working section of producing polycrystalline silicon in the prior art.
The invention is realized by the following technical scheme:
a method for controlling the content of dichlorosilane in refined trichlorosilane comprises the following steps:
feeding the synthesized high-purity trichlorosilane and the recovered trichlorosilane into a separation tower for mixing,
heating a separation tower to vaporize chlorosilane, condensing dichlorosilane to a liquid state through a condenser, extracting part of the dichlorosilane, sending the rest part of the dichlorosilane back to the separation tower to be used as reflux liquid,
and acquiring a pressure value and a temperature value in the tower kettle of the separation tower, judging the relation between the content of the dichlorosilane in the separation tower and the pressure value and the temperature value of the separation tower through a DCS (distributed control System), and determining the extraction amount of the dichlorosilane.
Further, the trichlorosilane is high-purity trichlorosilane from a trichlorosilane synthesis working section and trichlorosilane containing 8-15% of dichlorosilane after rectification treatment.
Further, fitting according to gas-liquid balance data of trichlorosilane and dichlorosilane in the separation tower by adopting Aspen software to obtain the following relation among the content of dichlorosilane in the separation tower, the pressure value and the temperature value of the separation tower:
c (dichlorosilane) = (a multiplied by Pi-b) multiplied by Ln (Ti) + (C multiplied by Pi + d), wherein a, b and C are fitting parameters, Pi is a gas phase pressure value of a tower bottom of the separation tower, and Ti is a liquid phase temperature value of the tower bottom of the separation tower.
The utility model provides a system for controlling dichlorosilane content in refined trichlorosilane, including knockout tower and DCS system, the tower cauldron of knockout tower is equipped with thermometer and pressure gauge, be connected with synthetic trichlorosilane pipeline and retrieve trichlorosilane pipeline on the knockout tower, the top of the tower of knockout tower passes through pipeline I and connects the storage tank, be connected with dichlorosilane extraction pipeline on the storage tank, be equipped with valve I on the dichlorosilane extraction pipeline, the storage tank passes through backflow pipeline and is connected with knockout tower upper portion, the tower cauldron of knockout tower is connected with refined trichlorosilane pipeline, the DCS system respectively with the thermometer, the pressure gauge, valve I control connection, the tower cauldron of knockout tower is connected with the reboiler, be equipped with the condenser on the pipeline that knockout tower and storage tank are connected.
Furthermore, a booster pump I is arranged on a dichlorosilane extraction pipeline connected with the storage tank; a booster pump II is arranged on the refined trichlorosilane pipeline.
Furthermore, the booster pump I and the booster pump II both use a shield pump.
Furthermore, a valve II is arranged on the return pipeline, and a valve III is arranged on the refined trichlorosilane pipeline
Compared with the prior art, the invention has the following advantages and beneficial effects:
according to the invention, the content of dichlorosilane in the refined trichlorosilane can be accurately controlled in real time by adopting the method, so that the control stability of the reduction furnace is improved, the quality of a polycrystalline silicon product can be improved, the densification rate of the polycrystalline silicon is improved by 8-12%, the power consumption of a reduction section is reduced by about 10%, and the cost of per ton of polycrystalline silicon is saved by over 1000 yuan.
In the invention, the recovered trichlorosilane obtained after the treatment of the rectifying section in the production process of the polycrystalline silicon can be recycled, and the recovered trichlorosilane contains 8-15% of dichlorosilane, so that the aims of saving energy and reducing consumption are fulfilled.
Thirdly, according to the invention, by combining with Aspen software, gas-liquid balance data of trichlorosilane and dichlorosilane in the separation tower are obtained and fitted to obtain the relation between the content of dichlorosilane in the separation tower and the pressure value and the temperature value at the bottom of the separation tower, the relation can be used for referring to the extraction value of given dichlorosilane, adjusting the extraction amount of dichlorosilane in real time, and ensuring that the content of dichlorosilane in the refined trichlorosilane obtained by the whole system is stable, thereby improving the overall quality of products.
Fourthly, the invention also provides a system for controlling the content of the dichlorosilane in the refined trichlorosilane which is matched with the method, and the device, the pipeline, the instrument and the like have reasonable design and can ensure the stable operation of the system.
In the invention, a tower kettle of the separation tower is connected with a shell-and-tube heat exchanger, and can also be heated by saturated steam or chlorosilane steam at the top of other rectifying towers.
Sixthly, a booster pump I is arranged on a dichlorosilane extraction pipeline connected with the storage tank and used for pumping liquid-phase dichlorosilane to the next working procedure; the booster pump II is arranged on the refined trichlorosilane pipeline to ensure that the refined trichlorosilane is output as expected, and the booster pump I and the booster pump II both adopt shielding pumps to ensure that materials cannot be leaked.
Seventhly, in the invention, the return pipeline is provided with a valve II, the refined trichlorosilane pipeline is provided with a valve III, and the refined trichlorosilane component content is ensured to be within a stable range and the quality of finished products is ensured by controlling the opening degree of the valve II and the valve III.
Drawings
Fig. 1 is a schematic system configuration diagram of embodiment 4.
Wherein, 1, a separation tower; 2. a DCS system; 3. a thermometer; 4. a pressure gauge; 5. a pipeline for synthesizing trichlorosilane; 6. a pipeline for recovering trichlorosilane; 7. a line I; 8. a storage tank; 9. a dichlorosilane extraction pipeline; 10. a valve I; 11. a return line; 12. a pipeline for refining trichlorosilane; 13. a shell-and-tube heat exchanger; 14. a condenser; 15. a booster pump I; 16. a booster pump II; 17. a valve II; 18. a valve III; 1.1, tower top; 1.2, tower bottom.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
A method for controlling the content of dichlorosilane in refined trichlorosilane belongs to the technical field of polysilicon production, and comprises the following steps:
feeding the synthesized high-purity trichlorosilane and the recovered trichlorosilane into a separation tower for mixing,
heating the separation tower to vaporize dichlorosilane in chlorosilane, condensing the dichlorosilane to liquid state, extracting part of the dichlorosilane, sending the rest part of the dichlorosilane back to the separation tower,
and acquiring a pressure value and a temperature value in the separation tower, judging the relation between the content of the dichlorosilane in the separation tower and the pressure value and the temperature value in the separation tower through a DCS (distributed control System), and determining the extraction quantity of the dichlorosilane.
Example 2
The embodiment is further optimized in embodiment 1, and the difference is that the trichlorosilane comes from high-purity trichlorosilane in a trichlorosilane synthesis working section and trichlorosilane containing 8-15% dichlorosilane after rectification treatment.
Example 3
Compared with the embodiment 1-2, the difference is that Aspen software is adopted, and fitting is carried out according to gas-liquid balance data of trichlorosilane and dichlorosilane in the separation tower to obtain the following relation among the content of dichlorosilane in the separation tower, the pressure value and the temperature value at the bottom of the separation tower:
c (dichlorosilane) = (a multiplied by Pi-b) × Ln (Ti) + (C multiplied by Pi + d), wherein a, b and C are fitting parameters, Pi is a gas phase pressure value of a tower bottom of the separation tower, and Ti is a liquid phase temperature value of the tower bottom of the separation tower.
Example 4
This embodiment is to illustrate the present technical solution, and further illustrates the technical solution by taking a production line of 5 ten thousand tons of polysilicon produced in one year by this company as an example.
In this embodiment, referring to fig. 1, the system for controlling the content of dichlorosilane in refined trichlorosilane specifically includes a separation tower 1 and a DCS system 2, the diameter of the separation tower 1 is about 3.6 meters, the height of the separation tower 1 is about 70 meters, the processing capacity of trichlorosilane is about 300 tons/h, the separation tower 1 may adopt a packed tower or a plate tower, and the embodiment adopts a plate tower.
A temperature gauge 3 and a pressure gauge 4 are arranged at a tower kettle 1.2 of the separation tower 1, the temperature gauge 3 is used for measuring the liquid phase temperature of the tower kettle 1.2, the pressure gauge 4 is used for measuring the gas phase pressure of the tower kettle 1.2, a synthetic trichlorosilane pipeline 5 and a trichlorosilane recovery pipeline 6 are connected to the separation tower 1, the tower top 1.1 of the separation tower 1 is connected with a storage tank 8 through a pipeline I7, a dichlorosilane extraction pipeline 9 is connected to the storage tank 8, a valve I10 is arranged on the dichlorosilane extraction pipeline 9, a valve I10 is a corrugated pipe adjusting valve, the storage tank 8 is made of 316L material, the volume is 50m3, a liquid level meter is arranged on the storage tank 8, the storage tank 8 is connected with the upper part of the separation tower 1 through a backflow pipeline 11, the tower kettle 1.2 of the separation tower 1 is connected with a refined trichlorosilane pipeline 12, a shell and tube system 2 is respectively connected with the temperature gauge 3, the pressure gauge 4 and the valve I10 in a control mode, the tower kettle 1.2 of the separation tower 1 is connected with a heat exchanger 13, the shell-and-tube heat exchanger 13 is preferably a reboiler, and a condenser 14 is provided on a pipeline connecting the separation column 1 and the storage tank 8.
Preferably, a booster pump I15 is arranged on the dichlorosilane extraction pipeline 9 connected with the storage tank 8; the refined trichlorosilane pipeline 12 is provided with a booster pump II16, and the booster pump I15 and the booster pump II16 are preferably shielding pumps.
Preferably, a valve II17 is arranged on the return line 11, and a valve III18 is arranged on the refined trichlorosilane line 12.
Specifically, the method for controlling the content of dichlorosilane in the refined trichlorosilane comprises the following steps:
conveying trichlorosilane with the purity of 100% from a trichlorosilane synthesis working section and trichlorosilane containing 8% -15% dichlorosilane from a recovery rectification working section into a separation tower 1 for mixing,
the separation tower 1 is heated by a reboiler, the mixture of trichlorosilane and dichlorosilane in a vaporization tower kettle 1.2 is subjected to heat transfer and mass transfer with reflux liquid from a tower top 1.1 part in the ascending process of vaporized steam in the separation tower 1 on a tower plate, the gas phase is converted into pure dichlorosilane after reaching the tower top 1.1, the pure dichlorosilane is condensed into liquid dichlorosilane by a condenser 14 and enters a reflux tank, part of dichlorosilane is extracted through an extraction pipeline at the tower top 1.1, and the rest part of dichlorosilane is returned to the separation tower 1 as reflux liquid,
the DCS 2 acquires the pressure value of the gas phase 1.2 in the tower kettle 1 of the separation tower 1 and the temperature value of the liquid phase 1.2 in the tower kettle in real time, and the DCS 2 calculates the concentration of dichlorosilane in the trichlorosilane in the tower kettle 1.2 of the separation tower 1 according to a set concentration formula of dichlorosilane. In the scheme, the calculation formula of the concentration of dichlorosilane adopts Aspen software, and fitting is carried out according to gas-liquid balance data of trichlorosilane and dichlorosilane to obtain a formula of the content of dichlorosilane and the temperature and pressure:
c (dichlorosilane) = (a multiplied by Pi-b) multiplied by Ln (Ti) + (C multiplied by Pi + d), wherein a, b and C are fitting parameters, Pi is a gas phase pressure value of a tower bottom of the separation tower, and Ti is a liquid phase temperature value of the tower bottom of the separation tower.
And determining the extraction amount of dichlorosilane at the tower top according to the downstream requirement on the content of dichlorosilane in the refined trichlorosilane.
Table 1 is a statistical table of the production of polysilicon in different time periods in the production line, the product condition and the production energy consumption condition, and the statistical time is the operation data of selecting the same production line at intervals of 3 days.
TABLE 1
Figure DEST_PATH_IMAGE001
As can be seen from Table 1, the system can control the fluctuation of the concentration of dichlorosilane in the refined trichlorosilane within the range of +/-0.1 percent, while the traditional process can only control the fluctuation within the range of 0.5 percent. The stable control of the concentration of dichlorosilane in the refined trichlorosilane plays a great role in the stable operation of the reduction furnace.
Compared with the prior preparation technology, the polycrystalline silicon product obtained by the scheme can improve the densification rate of the polycrystalline silicon product by 8-12%, and the data in Table 1 show that the product densification can reach 67% and the reduction power consumption is reduced by more than 10%. By taking a device for producing 5 ten thousand tons of polysilicon annually as an example, after the scheme of the invention is adopted, the densification rate of a polysilicon product is improved to 65 percent from the original 55 percent, the reduction power consumption is reduced to 40 kW.h/kg from the original 44 kW.h/kg, the price of the polysilicon densified material is 1 ten thousand yuan higher than that of silicon materials with other qualities per ton, and the power price is 0.35 yuan per degree, so that the benefit created all the year round is about: 50000 tons multiplied by 10% multiplied by 1 ten thousand yuan/ton +50000 tons multiplied by 4 kW.h/kg multiplied by 0.35 multiplied by 1000 div 10000=12000 ten thousand yuan, and the production cost of an enterprise is obviously reduced.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modifications and equivalent variations of the above embodiment according to the technical spirit of the present invention are within the scope of the present invention.

Claims (7)

1. A method for controlling the content of dichlorosilane in refined trichlorosilane is characterized by comprising the following steps:
feeding the synthesized high-purity trichlorosilane and the recovered trichlorosilane into a separation tower for mixing,
heating a separation tower to vaporize chlorosilane, condensing dichlorosilane to a liquid state through a condenser, extracting part of the dichlorosilane, sending the rest part of the dichlorosilane back to the separation tower to be used as reflux liquid,
and acquiring a pressure value and a temperature value in the tower kettle of the separation tower, judging the relation between the content of the dichlorosilane in the separation tower and the pressure value and the temperature value of the separation tower through a DCS (distributed control System), and determining the extraction amount of the dichlorosilane.
2. The method for controlling the content of dichlorosilane in refined trichlorosilane according to claim 1, which is characterized by comprising the following steps: the trichlorosilane is high-purity trichlorosilane from a trichlorosilane synthesis working section and trichlorosilane containing 8-15% of dichlorosilane after rectification treatment.
3. The method for controlling the content of dichlorosilane in refined trichlorosilane according to claim 1, which is characterized by comprising the following steps: fitting according to gas-liquid balance data of trichlorosilane and dichlorosilane in the separation tower by adopting Aspen software to obtain the following relation among the content of dichlorosilane in the separation tower, the pressure value and the temperature value at the bottom of the separation tower:
c (dichlorosilane) = (a multiplied by Pi-b) multiplied by Ln (Ti) + (C multiplied by Pi + d), wherein a, b and C are fitting parameters, Pi is a gas phase pressure value of a tower bottom of the separation tower, and Ti is a liquid phase temperature value of the tower bottom of the separation tower.
4. A system for controlling the content of dichlorosilane in the refined trichlorosilane is characterized in that: the device comprises a separation tower and a DCS (distributed control system), a temperature meter and a pressure meter are arranged at a tower kettle of the separation tower, a synthetic trichlorosilane pipeline and a trichlorosilane recycling pipeline are connected to the separation tower, the tower top of the separation tower is connected with a storage tank through a pipeline I, a dichlorosilane extraction pipeline is connected to the storage tank, a valve I is arranged on the dichlorosilane extraction pipeline, the storage tank is connected with the upper part of the separation tower through a backflow pipeline, the tower kettle of the separation tower is connected with a refined trichlorosilane pipeline, the DCS is respectively connected with the temperature meter, the pressure meter and the valve I in a control mode, the tower kettle of the separation tower is connected with a shell-and-tube heat exchanger, and a condenser is arranged on a pipeline connected with the storage tank.
5. The system for controlling the content of dichlorosilane in refined trichlorosilane according to claim 4, wherein the system comprises: a booster pump I is arranged on a dichlorosilane extraction pipeline connected with the storage tank; a booster pump II is arranged on the refined trichlorosilane pipeline.
6. The system for controlling the content of dichlorosilane in the refined trichlorosilane according to claim 5, wherein the system comprises: and the booster pump I and the booster pump II are both provided with shielding pumps.
7. The system for controlling the content of dichlorosilane in refined trichlorosilane according to claim 4, wherein the system comprises: a valve II is arranged on the return pipeline, and a valve III is arranged on the refined trichlorosilane pipeline.
CN202210702339.0A 2022-06-21 2022-06-21 Method and system for controlling content of dichlorosilane in refined trichlorosilane Pending CN115092934A (en)

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