CN113171629A - Trichlorosilane differential pressure coupling rectification process and dynamic control scheme - Google Patents
Trichlorosilane differential pressure coupling rectification process and dynamic control scheme Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
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- C—CHEMISTRY; METALLURGY
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- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10778—Purification
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Abstract
The invention belongs to the field of purification in the chemical industry, and relates to a trichlorosilane differential pressure coupling rectification process and a dynamic control scheme. The method comprises the following steps: a flow controller for controlling the feed flow rate; the pressure controller is used for controlling the tower pressure of the rectifying tower; the liquid level controller is used for controlling the liquid levels of the tower top reflux tank and the tower kettle; the temperature controller is used for adjusting the tower temperature of the rectifying tower; and the proportion controller is respectively used for fixing the ratio of the reflux quantity of the low-pressure tower to the feeding flow, the ratio of the heat load of the reboiler of the high-pressure tower to the feeding flow and the ratio of the reflux quantity of the high-pressure tower to the extraction quantity at the top of the tower. The technological process of the invention realizes heat integration, greatly reduces energy consumption; the dynamic control scheme can robustly control the feed flow disturbance within 10 percent and the feed impurity disturbance of 25 percent, and the purity of the trichlorosilane product obtained by separation is more than 99.99 percent; has stronger robustness and stability.
Description
Technical Field
The invention belongs to the field of purification in the chemical industry, and particularly relates to a trichlorosilane differential pressure coupling rectification process method and a dynamic control scheme, which are particularly suitable for dynamic control of a differential pressure coupling rectification process with similar mixture boiling points and extremely high product purity.
Background
The polycrystalline silicon is used as a basic material in the photovoltaic industry and the integrated circuit industry, and plays an important role in the industries such as mobile communication, new energy automobiles and the like. The trichlorosilane is used as an intermediate product for producing the polycrystalline silicon by the improved Siemens method, and the purity of the trichlorosilane is one of the factors influencing the quality of the polycrystalline silicon. The trichlorosilane refining process mostly adopts a multistage rectification technology, the number of rectification stages is multiple, the number of tower plates is large, the reflux ratio is large, and a large amount of steam and electric energy are consumed. Generally, the differential pressure coupling technology can recover waste heat and reduce energy consumption, so that the differential pressure coupling rectification technology is applied to the trichlorosilane refining process.
The dynamic control plays an important role in starting the vehicle quickly and without faults, reducing the number of defective products and ensuring safe operation. In the double-tower differential pressure coupling rectification process, the integration of energy reduces the control freedom degree, the interaction between the two towers is stronger, and the control difficulty is increased, so the invention provides an effective control scheme mainly aiming at the steady flow of the trichlorosilane differential pressure coupling rectification process, and ensures the quality of high-purity trichlorosilane products and the stable operation of the device.
A patent (CN102649019A) discloses a trichlorosilane rectification system, and the method provides the trichlorosilane rectification system which can improve the quality of a trichlorosilane product and has low energy consumption and small equipment investment, but the patent does not realize dynamic control.
The patent (CN1962014A) discloses a general model control system for high-purity rectification, which is suitable for the rectification and purification process of high-purity products, but a specific separation system is not given, the patent gives a control strategy for single-tower rectification, and compared with the trichlorosilane differential pressure coupling rectification control of the patent, the single-tower control variables are few, the coupling degree among the variables is small, and the difficulty is lower than that of the patent.
Disclosure of Invention
[ problem to be solved ]
Aiming at the technical characteristics of the trichlorosilane rectification process, the invention provides a dynamic control scheme of a trichlorosilane differential pressure coupling rectification process, which aims to solve the scientific problems as follows:
the invention aims to provide a dynamic control scheme suitable for a differential pressure coupling rectification process.
The invention also aims to provide application of the control scheme in a trichlorosilane purification process.
[ solution ]
The technical scheme of the invention is as follows: a trichlorosilane differential pressure coupling rectification process and a dynamic control scheme are characterized in that the rectification process for separating a dichlorosilane-trichlorosilane-silicon tetrachloride ternary mixture is a double-tower differential pressure coupling rectification process, and the dynamic control scheme for the separation process of the dichlorosilane-trichlorosilane-silicon tetrachloride ternary mixture is a dynamic control scheme for the double-tower differential pressure coupling rectification process.
The double-tower differential pressure coupling separation process mainly comprises the following steps:
(1) and (3) a low-pressure tower rectification process: crude trichlorosilane from a cold hydrogenation device and an anti-disproportionation device enters a low-pressure tower T1 from the middle part, tower top steam is condensed by an E1 condenser and then enters a reflux tank D1, one part of the tower top steam returns to a low-pressure tower T1 through a pump P1, the other part of the tower top steam is extracted as a dichlorosilane product, one part of tower bottom liquid enters a heat exchanger E2 and then enters a low-pressure tower T1 after reboiling, and the other part of the tower bottom liquid enters a high-pressure tower T2 for secondary rectification;
(2) the high-pressure tower rectification process: materials from the bottom of a low-pressure tower T1 enter a high-pressure tower T2 from the middle part through a pump P2, a reboiler E3 heats the tower bottom liquid of the high-pressure tower T2, tower top steam enters a heat exchanger E2 hot material inflow port from a tower top gas phase outlet for heat exchange, the heat exchanged steam enters a reflux tank D2, one part of the materials in the reflux tank D2 reflows to the high-pressure tower T2 through the pump P3, the other part of the materials obtains a high-purity trichlorosilane product, and the tower bottom material flow obtains a silicon tetrachloride product;
(3) differential pressure coupling process: heat integration is realized in a heat exchanger E2, heat exchange is carried out between gas-phase trichlorosilane from the top of the high-pressure tower T2 and liquid phase from the bottom of the low-pressure tower T1, the gas-phase trichlorosilane is condensed, and heat is provided for the low-pressure tower T1.
The dynamic control scheme of the double-tower differential pressure coupling rectification process mainly comprises the following control structures:
a tower top pressure controller PC1, reflux tank liquid level controllers LC11 and LC21, tower bottom liquid level controllers LC12 and LC22, a low-pressure tower T1 feeding flow controller FC, a low-pressure tower T1 temperature controller TC1, a high-pressure tower T2 temperature controller TC2, a low-pressure tower T01 ratio controller R1/F, and a high-pressure tower T02 ratio controller QR2/F, RR 2;
the ratio controller R1/F of the low-pressure tower T1 is the ratio between the reflux quantity and the feed flow of the low-pressure tower T1, and the ratio controller QR2/F of the high-pressure tower T2 is the ratio between the reboiler heat load and the feed flow of the high-pressure tower T2.
The control behavior of the controller is as follows:
(1) the feeding amount of the low-pressure tower T1 is controlled by a flow controller FC, and the flow controller FC is controlled in the reverse direction;
(2) the overhead pressure of the low-pressure column T1 was controlled by the removal rate of the corresponding overhead condenser heat load, in reverse control by the pressure controller PC 1;
(3) the liquid levels of reflux tanks of the low-pressure tower T1 and the high-pressure tower T2 are controlled by adjusting the extraction amount at the top of the tower, and liquid level controllers LC11 and LC21 of the reflux tanks are in forward control; the liquid levels of the tower bottoms of the low-pressure tower T1 and the high-pressure tower T2 are controlled by adjusting the bottom extraction amount, and the tower bottom liquid level controllers LC12 and LC22 are in forward control;
(4) the ratio of the reflux quantity to the feeding flow of the low-pressure tower T2 is fixed through a ratio controller R1/F, the ratio of the heat load to the feeding flow of a reboiler of a high-pressure tower T2 is fixed through a ratio controller QR2/F, and the ratio of the reflux quantity to the overhead extraction quantity of the high-pressure tower T2 is fixed through a ratio controller RR 2;
(5) the temperature of the low-pressure tower T1 is controlled by controlling the temperature of the temperature sensitive plate in the low-pressure tower T1, and the temperature of the temperature sensitive plate in the low-pressure tower T1 is controlled by manipulating the QR2/F ratio; the temperature of the high-pressure tower T2 is controlled by controlling the temperature of a temperature sensitive plate in the high-pressure tower T2, and the temperature of the temperature sensitive plate in the high-pressure tower T2 is controlled by manipulating the value of RR 2;
the temperature sensitive plate is the most sensitive plate of temperature change in the rectifying tower, the temperature change of the plate in the rectifying tower is calculated by changing the heat load of a reboiler of the rectifying tower, and the position with the maximum temperature change is the temperature sensitive plate of the rectifying tower.
The control scheme can robustly control the feed flow disturbance within 10 percent and the feed impurity disturbance of 25 percent, and the purity of the trichlorosilane product obtained by separation is more than 99.99 percent.
[ advantageous effects ]
The invention has the following beneficial effects:
(1) the heat integration is realized in the process, the latent heat of the gas phase material flow at the top of the high-pressure tower provides energy for the low-pressure tower low-liquid reboiling, and the energy consumption is greatly reduced.
(2) The crude trichlorosilane from the cold hydrogenation and anti-disproportionation device is successfully separated and purified, and the high purity of the product trichlorosilane is ensured.
(3) The control structure can well solve the disturbance of the feeding flow and the feeding impurities.
(4) The steady dynamic control of the trichlorosilane double-tower differential pressure coupling rectification is realized.
Drawings
As will be further explained below in conjunction with the drawings,
FIG. 1 is a schematic structural diagram of the present invention.
A low-pressure tower T1, a high-pressure tower T2, valves V1-V9, pumps P1-P3, heat exchangers E1-E3 and tower top reflux tanks D1-D2; a PC1 top pressure controller, LC11 and LC21 top reflux tank liquid level controllers, LC12 and LC22 tower kettle liquid level controllers, an FC low-pressure tower feeding flow rate controller, TC1 and TC2 rectifying tower temperature controllers, R1/F is a ratio controller of a reflux quantity R1 and a feeding flow rate F of a fixed low-pressure tower T1, RR2 is a ratio controller of a reflux ratio of a fixed high-pressure tower T2, QR2/F is a ratio controller of a feeding flow rate F of a fixed low-pressure tower T1 and a tower bottom reboiler thermal load QR2 of a high-pressure tower T2, and Delta T is dead time; the solid line with arrows represents the logistics conduits and the dashed line with arrows represents the signals of the controller.
FIG. 2 is a graph of the dynamic response of a feed flow disturbance, with a solid line representing + 10% of the feed flow disturbance and a dashed line representing-10% of the feed flow disturbance.
FIG. 3 is a graph of the dynamic response of a feed impurity perturbation, with a solid line representing + 25% feed impurity perturbation and a dashed line representing-25% feed impurity perturbation.
Detailed Description
The following is further described with reference to fig. 1, but not to limit the scope of the invention.
The steady state process flow comprises the following steps: the feeding flow rate is 40000kg/h, the temperature is 40 ℃, the pressure is 500kPa, and the feed comprises 3% of dichlorosilane, 92% of trichlorosilane and 3% of silicon tetrachloride; the theoretical plate number of the low-pressure tower T1 is 84, the raw material liquid is introduced from the 24 th plate, and the operation pressure is 400 kPa; the theoretical plates of the high-pressure tower T2 are 60, the raw materials are also introduced from the 40 th plate, the operation pressure is 670kPa, under the process condition, the purity of trichlorosilane reaches more than 99.99 percent, and the purity of dichlorosilane and silicon tetrachloride reaches more than 99 percent.
Example 1:
the controllers are initialized to operate, set values are automatically input, the control range is reasonably determined, and a closed loop is used as a test method. The feed flow rate was changed from 40000kg/h to 44000kg/h, the dynamic response curve thereof is shown in FIG. 2 (solid line), the purity overshoot σ of dichlorosilane was 0.004, the adjustment time τ _ s was 2h, and the remainder e (∞) was 0.0001; the purity overshoot sigma of the trichlorosilane is 0.000058, the adjusting time is tau _ s for 4h, and the residual error e (∞) is-0.000009; the silicon tetrachloride purity overshoot sigma is 0.0096, the adjusting time is tau _ s is 4h, and the residual difference e (∞) is-0.00427; the temperature overshoot sigma of the high-pressure tower T2 is 16 ℃, the adjusting time is tau _ s for 4h, and the residual difference e (∞) is 0; indicating that the control process can handle disturbances of + 10% of the feed flow rate well.
Example 2:
the controllers are initialized to operate, set values are automatically input, the control range is reasonably determined, and a closed loop is used as a test method. The feeding flow rate is changed from 40000kg/h to 36000kg/h, the dynamic response curve is shown in figure 2 (dotted line), the purity overshoot sigma of the dichlorosilane is-0.0127, the adjusting time is tau _ s is 2h, and the residual difference e (∞) is-0.00012; the purity overshoot sigma of the trichlorosilane is-0.00019, the adjusting time is tau _ s for 4h, and the residual error e (∞) is 0.000006; the silicon tetrachloride purity overshoot sigma is-0.0542, the adjusting time is tau _ s for 4h, and the residual error e (∞) is 0.003; the temperature overshoot sigma of the high-pressure tower T2 is-15 ℃, the adjusting time is tau _ s for 4h, and the residual error e (∞) is 0; indicating that the control process can handle disturbances of-10% of the feed flow rate very well.
Example 3:
the controllers are initialized to operate, set values are automatically input, the control range is reasonably determined, and a closed loop is used as a test method. The feed composition comprises 4% of dichlorosilane, 92% of trichlorosilane, and 4% of silicon tetrachloride changed into 5% of dichlorosilane, 90% of trichlorosilane, and 5% of silicon tetrachloride, the dynamic response curve of which is shown in figure 3 (solid line), the purity overshoot sigma of dichlorosilane is 0.00046, the adjusting time tau _ s is 2.5h, and the residual error e (∞) is-0.00048; the purity overshoot sigma of the trichlorosilane is 0.000018, the adjusting time is tau _ s for 4h, and the residual error e (∞) is 0.000014; the silicon tetrachloride purity overshoot sigma is 0.0021, the adjusting time is tau _ s is 3h, and the residual difference e (∞) is-0.00056; the temperature overshoot sigma of the high-pressure tower T2 is 1.9 ℃, the adjusting time is tau _ s for 4h, and the residual error e (∞) is 0; indicating that the control process can handle disturbances of + 25% of the feed impurities well.
Example 4:
the controllers are initialized to operate, set values are automatically input, the control range is reasonably determined, and a closed loop is used as a test method. The feed composition comprises 4% of dichlorosilane, 92% of trichlorosilane, and 4% of silicon tetrachloride is changed into 3% of dichlorosilane, 94% of trichlorosilane, and 3% of silicon tetrachloride, the dynamic response curve of which is shown in figure 3 (solid line), the purity overshoot sigma of dichlorosilane is-0.0005, the adjusting time tau _ s is 2.5h, and the residual error e (∞) is 0.000454; the purity overshoot sigma of the trichlorosilane is-0.000018, the adjusting time is tau _ s for 4h, and the residual error e (∞) is-0.000008; the silicon tetrachloride purity overshoot sigma is-0.0026, the adjusting time is tau _ s is 3h, and the residual difference e (∞) is 0.000527; the temperature overshoot sigma of the high-pressure tower T2 is-1.8 ℃, the adjusting time is tau _ s for 4h, and the residual error e (∞) is 0; indicating that the control process can handle disturbances of-25% of the feed impurities well.
Claims (5)
1. A trichlorosilane differential pressure coupling rectification process and a dynamic control scheme are characterized in that the rectification process for separating a dichlorosilane-trichlorosilane-silicon tetrachloride ternary mixture is a double-tower differential pressure coupling rectification process, and the dynamic control scheme for the separation process of the dichlorosilane-trichlorosilane-silicon tetrachloride ternary mixture is a dynamic control scheme for the double-tower differential pressure coupling rectification process.
2. The method of claim 1, wherein the steady-state distillation process for separating the ternary mixture of dichlorosilane, trichlorosilane and silicon tetrachloride comprises the following steps:
(1) and (3) a low-pressure tower rectification process: crude trichlorosilane from a cold hydrogenation device and an anti-disproportionation device enters a low-pressure tower T1 from the middle part, tower top steam is condensed by an E1 condenser and then enters a reflux tank D1, one part of the tower top steam returns to a low-pressure tower T1 through a pump P1, the other part of the tower top steam is extracted as a dichlorosilane product, one part of tower bottom liquid enters a heat exchanger E2 and then enters a low-pressure tower T1 after reboiling, and the other part of the tower bottom liquid enters a high-pressure tower T2 for secondary rectification;
(2) the high-pressure tower rectification process: materials from the bottom of a low-pressure tower T1 enter a high-pressure tower T2 from the middle part through a pump P2, a reboiler E3 heats the tower bottom liquid of the high-pressure tower T2, tower top steam enters a heat exchanger E2 hot material inflow port from a tower top gas phase outlet for heat exchange, the heat exchanged steam enters a reflux tank D2, one part of the materials in the reflux tank D2 reflows to the high-pressure tower T2 through the pump P3, the other part of the materials obtains a high-purity trichlorosilane product, and the tower bottom material flow obtains a silicon tetrachloride product;
(3) differential pressure coupling process: heat integration is realized in a heat exchanger E2, heat exchange is carried out between gas-phase trichlorosilane from the top of the high-pressure tower T2 and liquid phase from the bottom of the low-pressure tower T1, the gas-phase trichlorosilane is condensed, and heat is provided for the low-pressure tower T1.
3. The method of claim 1, wherein the dynamic control scheme for controlling the process for separating the ternary mixture of dichlorosilane, trichlorosilane and silicon tetrachloride mainly comprises the following control structures:
a tower top pressure controller PC1, reflux tank liquid level controllers LC11 and LC21, tower bottom liquid level controllers LC12 and LC22, a low-pressure tower T1 feeding flow controller FC, a low-pressure tower T1 temperature controller TC1, a high-pressure tower T2 temperature controller TC2, a low-pressure tower T01 ratio controller R1/F, and a high-pressure tower T02 ratio controller QR2/F, RR 2;
the ratio controller R1/F of the low-pressure tower T1 is the ratio between the reflux quantity and the feed flow of the low-pressure tower T1, and the ratio controller QR2/F of the high-pressure tower T2 is the ratio between the reboiler heat load and the feed flow of the high-pressure tower T2.
4. A controller as claimed in claim 3, the control action being as follows:
(1) the feeding amount of the low-pressure tower T1 is controlled by a flow controller FC, and the flow controller FC is controlled in the reverse direction;
(2) the overhead pressure of the low-pressure column T1 was controlled by the removal rate of the corresponding overhead condenser heat load, in reverse control by the pressure controller PC 1;
(3) the liquid levels of reflux tanks of the low-pressure tower T1 and the high-pressure tower T2 are controlled by adjusting the extraction amount at the top of the tower, and liquid level controllers LC11 and LC21 of the reflux tanks are in forward control; the liquid levels of the tower bottoms of the low-pressure tower T1 and the high-pressure tower T2 are controlled by adjusting the bottom extraction amount, and the tower bottom liquid level controllers LC12 and LC22 are in forward control;
(4) the ratio of the reflux quantity to the feeding flow of the low-pressure tower T2 is fixed through a ratio controller R1/F, the ratio of the heat load to the feeding flow of a reboiler of a high-pressure tower T2 is fixed through a ratio controller QR2/F, and the ratio of the reflux quantity to the overhead extraction quantity of the high-pressure tower T2 is fixed through a ratio controller RR 2;
(5) the temperature of the low-pressure tower T1 is controlled by controlling the temperature of the temperature sensitive plate in the low-pressure tower T1, and the temperature of the temperature sensitive plate in the low-pressure tower T1 is controlled by manipulating the QR2/F ratio; the temperature of the high-pressure tower T2 is controlled by controlling the temperature of a temperature sensitive plate in the high-pressure tower T2, and the temperature of the temperature sensitive plate in the high-pressure tower T2 is controlled by manipulating the value of RR 2;
the temperature sensitive plate is the most sensitive plate of temperature change in the rectifying tower, the temperature change of the plate in the rectifying tower is calculated by changing the heat load of a reboiler of the rectifying tower, and the position with the maximum temperature change is the temperature sensitive plate of the rectifying tower.
5. The trichlorosilane differential pressure coupling rectification process according to claim 1, which is characterized in that: the method can robustly control the feed flow disturbance within 10 percent and the feed impurity disturbance of 25 percent, and the purity of the trichlorosilane product obtained by separation is more than 99.99 percent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116135277A (en) * | 2023-03-22 | 2023-05-19 | 南京工业大学 | Electrically driven variable pressure rectification device and control method |
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| CN203754433U (en) * | 2014-03-31 | 2014-08-06 | 中国恩菲工程技术有限公司 | Polycrystalline silicon preparation device |
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| US3415720A (en) * | 1964-10-28 | 1968-12-10 | Shell Oil Co | Apparatus for the automatic control of a continuous distillation operation for maintaining a constant ratio of bottom product flow to heat input flow |
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| CN203754433U (en) * | 2014-03-31 | 2014-08-06 | 中国恩菲工程技术有限公司 | Polycrystalline silicon preparation device |
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| CN116135277A (en) * | 2023-03-22 | 2023-05-19 | 南京工业大学 | Electrically driven variable pressure rectification device and control method |
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