An automated rectification system for triisopropylsilane and its control method

Abstract

The present invention discloses an automated rectification system for triisopropylsilane and its control method, specifically relating to the technical field of extracting triisopropylsilane. The system includes a crude product storage tank, a rectification kettle, a rectification column, a condensation unit, a reflux ratio regulator, a pre-fraction receiving tank, a solvent receiving tank, a transitional fraction tank, a product receiving tank, and a vacuum unit; the method includes (1) feeding; (2) pre-fraction receiving; (3) solvent receiving; (4) transitional fraction receiving; (5) product receiving. Beneficial effects: The present invention provides an automated rectification system for triisopropylsilane and its control method, realizing one-key startup of the system, without the need for personnel operation in the on-site operation state, reducing the frequency of personnel operation in triisopropylsilane rectification and reducing production costs; realizing automated process operation and being able to continuously and stably execute to produce qualified triisopropylsilane products.

Description

Technical Field

[0001] This invention patent relates to the technical field of extracting triisopropylsilane, and specifically relates to an automatic rectification system for triisopropylsilane and its control method. Background Art

[0002] Triisopropylsilane is a chemical intermediate, which can be used for synthesizing sterically hindered organosilicon protecting agents, preparing special organosilicon materials and organic synthesis. It is an excellent hydrogen proton donor and is applied to many reduction reactions. Currently, the patent with the publication number CN103204869B discloses a patent for a synthesis method of high-purity triisopropylsilane, which discloses that magnesium, a solvent, 2-chloropropane, methylcyclohexane, and trichlorosilane are used as raw materials for reaction, and then triisopropylsilane is obtained through vacuum distillation; currently, vacuum distillation generally includes rough distillation and rectification, and the rectification is manually controlled, so there are problems such as unstable control process and large fluctuations, ultimately affecting the output and quality of the product. Summary of the Invention

[0003] The purpose of the present invention is to provide an automatic rectification system for triisopropylsilane and its control method that realizes automatic process operation and reduces production costs.

[0004] The first purpose of the present invention is implemented by the following technical solution: an automatic rectification system for triisopropylsilane, which includes a crude product storage tank, a rectification kettle, a rectification column, a condensation unit, a reflux ratio regulator, a pre-fraction receiving tank, a solvent receiving tank, a transition fraction tank, a product receiving tank, and a vacuum unit;

[0005] The liquid outlet of the crude product storage tank is communicated with the liquid inlet of the rectification kettle through a feed pipe, and a transfer pump and a feed valve are sequentially arranged on the feed pipe; a first liquid level sensor and a first temperature sensor are arranged in the rectification kettle;

[0006] The rectification column is communicated and arranged above the rectification kettle, the gas outlet at the top of the rectification column is communicated with the gas inlet of the condensation unit, and the gas outlet of the condensation unit is communicated with the gas inlet of the vacuum unit; a second temperature sensor is arranged at the top inside the rectification column; a pressure sensor is arranged inside the rectification column;

[0007] The condensate outlet of the condensation unit is communicated with the liquid inlet of the reflux ratio regulator, and the two liquid outlets of the reflux ratio regulator are respectively communicated with the liquid inlet above the rectification column and the liquid inlet end of the total liquid outlet pipe;

[0008] The liquid outlet end of the total liquid outlet pipe is respectively communicated with the liquid inlets of the pre-fraction receiving tank, the solvent receiving tank, the intermediate fraction tank and the product receiving tank; a pre-fraction inlet valve is arranged at the liquid inlet of the pre-fraction receiving tank; a solvent inlet valve is arranged at the liquid inlet of the solvent receiving tank; an intermediate fraction inlet valve is arranged at the liquid inlet of the intermediate fraction tank; a product inlet valve is arranged at the liquid inlet of the product receiving tank;

[0009] The top gas outlets of the pre-fraction receiving tank, the solvent receiving tank, the intermediate fraction tank and the product receiving tank are all communicated with the gas inlet of the vacuum unit; a pre-fraction gas outlet valve is arranged at the gas outlet of the pre-fraction receiving tank; a solvent gas outlet valve is arranged at the gas outlet of the solvent receiving tank; an intermediate fraction gas outlet valve is arranged at the gas outlet of the intermediate fraction tank; a product gas outlet valve is arranged at the gas outlet of the product receiving tank;

[0010] The gas outlet end of the steam pipeline is communicated with the gas inlet of the jacket of the distillation kettle; a steam cut-off valve is arranged at the gas inlet of the jacket;

[0011] The signal output ends of the first liquid level sensor, the first temperature sensor, the second temperature sensor and the pressure sensor are all signal-connected to the signal input end of the controller; the signal output end of the controller is respectively signal-connected to the signal input ends of the transfer pump, the feed valve, the vacuum unit, the reflux ratio regulator, the pre-fraction inlet valve, the solvent inlet valve, the intermediate fraction inlet valve, the product inlet valve, the pre-fraction gas outlet valve, the solvent gas outlet valve, the intermediate fraction gas outlet valve, the product gas outlet valve and the steam cut-off valve.

[0012] Further, the water outlet end of the circulating water pipeline is communicated with the water inlet of the jacket of the distillation kettle; a circulating water cut-off valve is arranged at the water inlet of the jacket;

[0013] The gas outlet end of the nitrogen pipeline is communicated with the gas inlet of the distillation kettle, and a nitrogen cut-off valve is arranged at the gas inlet of the distillation kettle;

[0014] The signal output end of the controller is respectively signal-connected to the signal input ends of the circulating water cut-off valve and the nitrogen cut-off valve.

[0015] Further, a second liquid level sensor is arranged in the crude product storage tank, and the signal output end of the second liquid level sensor is signal-connected to the signal input end of the controller.

[0016] Further, the vacuum unit is a Roots vacuum unit.

[0017] Further, the condensation unit includes a water cooler and a salt cooler. The gas outlet of the rectification column is communicated with the inlet of the water cooler. The outlet of the water cooler is communicated with the inlet of the salt cooler. The outlet of the salt cooler is communicated with the inlet of the vacuum unit. The condensate outlets of the water cooler and the salt cooler are both communicated with the inlet of the reflux ratio regulator.

[0018] Further, it further includes a residue storage tank. The liquid outlet of the rectification kettle is communicated with the inlet of the residue storage tank through a discharge pipe. A discharge valve and a residue discharge pump are sequentially arranged on the discharge pipe. The signal output end of the controller is respectively connected with the signal input ends of the discharge valve and the residue discharge pump through signals.

[0019] The second object of the present invention is implemented by the following technical solution: A control method for an automatic rectification system of triisopropylsilane, which includes the following steps:

[0020] (1) Feeding: Start with one key, the transfer pump starts to run, and at the same time the feed valve opens, and the crude product enters the rectification kettle. When the liquid level in the rectification kettle reaches the upper limit value, the controller controls the transfer pump and the feed valve to close.

[0021] (2) Receiving of the fore-fraction: After completing step (1), the controller controls the vacuum unit to start, and at the same time opens the steam cut-off valve. When the pressure in the rectification column < -0.09 MPa, control the reflux ratio regulator to open. All the condensate condensed by the condensation unit flows back into the rectification column, and the reflux time is 1 - 2 h. Then control the reflux ratio regulator to adjust the reflux ratio of the condensate flowing back into the rectification column and the condensate taken out into the fore-fraction receiving tank to 30:1. At the same time, open the fore-fraction inlet valve and the fore-fraction outlet valve.

[0022] (3) Solvent receiving: When the temperature at the top of the rectification column in step (2) rises to 80 °C, and the difference between the temperature at the top of the rectification column and the temperature in the rectification kettle < 10 °C, the controller controls the fore-fraction inlet valve and the fore-fraction outlet valve to close. At the same time, open the solvent inlet valve and the solvent outlet valve, and control the reflux ratio regulator to adjust the reflux ratio of the condensate flowing back into the rectification column and the condensate taken out into the solvent receiving tank to 10:6.

[0023] (4) Receiving of the transition fraction: When the temperature at the top of the rectification column in step (3) rises to 85 °C, the controller controls the solvent inlet valve and the solvent outlet valve to close, and controls the transition fraction inlet valve and the transition fraction outlet valve to open. At the same time, control the reflux ratio regulator to adjust the reflux ratio of the condensate flowing back into the rectification column and the condensate taken out into the transition fraction tank to 40:1.

[0024] (5)Product reception: When the temperature at the top of the rectification column in step (4) rises to 87 °C, the controller controls the closing of the transitional fraction inlet valve and the transitional fraction outlet valve, and controls the opening of the product inlet valve and the product outlet valve. At the same time, the controller controls the reflux ratio regulator to adjust the reflux ratio of the condensate flowing back to the rectification column and the condensate drawn into the product receiving tank to 10:8. When the temperature at the top of the rectification column rises to 90 °C, the controller controls the closing of the product inlet valve and the product outlet valve. At the same time, the controller controls the reflux ratio regulator to adjust so that all the condensate flows back into the rectification column, and controls the closing of the steam cut-off valve.

[0025] Furthermore, in step (1), when the liquid level in the crude product storage tank reaches the lower limit value, the controller controls the closing of the transfer pump and the feed valve.

[0026] Furthermore, after step (5), it also includes cooling down: The controller controls the opening of the circulating water cut-off valve to introduce cooling water for cooling. When the temperature in the rectification still cools down to below 40 °C, the controller controls the closing of the vacuum unit and the reflux ratio regulator.

[0027] Furthermore, after completing the cooling down, discharging is carried out. The controller controls the opening of the nitrogen cut-off valve to pressurize the rectification still to atmospheric pressure and then closes the nitrogen cut-off valve. After that, the controller controls the opening of the discharge valve and the operation of the still residue discharge pump to convey the still residue in the rectification still to the still residue storage tank. After the still residue in the rectification still is completely discharged, the controller controls the closing of the discharge valve and the still residue discharge pump.

[0028] Advantages of the present invention:

[0029] 1. The present invention provides an automated rectification system for triisopropylsilane, realizing one-key startup of the system. The on-site operation status does not require manual operation, reducing the frequency of personnel operating the rectification of triisopropylsilane and reducing the production cost.

[0030] 2. The present invention provides a control method for an automated rectification system of triisopropylsilane. Based on the set process parameters, judgment control operations are carried out, realizing automated process operation and being able to continuously and stably execute to produce qualified triisopropylsilane products. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the following drawings are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0032] Figure 1 It is the process system diagram of Embodiment 1 of the present invention.

[0033] Figure 2This is the control flow chart of Embodiment 1 of the present invention.

[0034] Crude product storage tank 1, rectifying kettle 2, jacket 201, rectifying column 3, condensation unit 4, water cooler 41, salt cooler 42, reflux ratio regulator 5, fore-fraction receiving tank 6, solvent receiving tank 7, intermediate fraction tank 8, product receiving tank 9, vacuum unit 10, feed pipe 11, transfer pump 12, feed valve 13, first liquid level sensor 14, first temperature sensor 15, second liquid level sensor 16, second temperature sensor 17, pressure sensor 18, liquid outlet main pipe 19, fore-fraction inlet valve 20, solvent inlet valve 21, intermediate fraction inlet valve 22, product inlet valve 23, fore-fraction gas outlet valve 24, solvent gas outlet valve 25, intermediate fraction gas outlet valve 26, product gas outlet valve 27, steam pipeline 28, steam cut-off valve 29, circulating water pipeline 30, circulating water cut-off valve 31, nitrogen pipeline 32, nitrogen cut-off valve 33, controller 34, residue storage tank 35, discharge pipe 36, discharge valve 37, residue discharge pump 38. Detailed implementation mode

[0035] The present invention will be further described in detail below through embodiments.

[0036] Embodiment 1: As Figure 1 shown, an automated rectification system for triisopropylsilane includes a crude product storage tank 1, a rectifying kettle 2, a rectifying column 3, a condensation unit 4, a reflux ratio regulator 5, a fore-fraction receiving tank 6, a solvent receiving tank 7, an intermediate fraction tank 8, a product receiving tank 9, a vacuum unit 10, and a residue storage tank 35; the liquid outlet of the crude product storage tank 1 is communicated with the liquid inlet of the rectifying kettle 2 through a feed pipe 11, and a transfer pump 12 and a feed valve 13 are sequentially arranged on the feed pipe 11; a first liquid level sensor 14 and a first temperature sensor 15 are arranged in the rectifying kettle 2; a second liquid level sensor 16 is arranged in the crude product storage tank 1; a rectifying column 3 is communicated above the rectifying kettle 2, the gas outlet at the top of the rectifying column 3 is communicated with the gas inlet of the condensation unit 4, the gas outlet of the condensation unit 4 is communicated with the gas inlet of the vacuum unit 10, and the vacuum unit 10 is a Roots vacuum unit 10; a second temperature sensor 17 is arranged at the top inside the rectifying column 3; a pressure sensor 18 is arranged inside the rectifying column 3.

[0037] The condensate outlet of the condensation unit 4 is communicated with the liquid inlet of the reflux ratio regulator 5. The two liquid outlets of the reflux ratio regulator 5 are respectively communicated with the liquid inlet above the rectification column 3 and the liquid inlet end of the total liquid outlet pipe 19. The liquid outlet end of the total liquid outlet pipe 19 is respectively communicated with the inlets of the fore-fraction receiving tank 6, the solvent receiving tank 7, the intermediate fraction tank 8 and the product receiving tank 9. A fore-fraction inlet valve 20 is arranged at the liquid inlet of the fore-fraction receiving tank 6. A solvent inlet valve 21 is arranged at the liquid inlet of the solvent receiving tank 7. An intermediate fraction inlet valve 22 is arranged at the liquid inlet of the intermediate fraction tank 8. A product inlet valve 23 is arranged at the liquid inlet of the product receiving tank 9. The top gas outlets of the fore-fraction receiving tank 6, the solvent receiving tank 7, the intermediate fraction tank 8 and the product receiving tank 9 are all communicated with the gas inlet of the vacuum unit 10. A fore-fraction gas outlet valve 24 is arranged at the gas outlet of the fore-fraction receiving tank 6. A solvent gas outlet valve 25 is arranged at the gas outlet of the solvent receiving tank 7. An intermediate fraction gas outlet valve 26 is arranged at the gas outlet of the intermediate fraction tank 8. A product gas outlet valve 27 is arranged at the gas outlet of the product receiving tank 9.

[0038] The gas outlet end of the steam pipeline 28 is communicated with the gas inlet of the jacket 201 of the rectification kettle 2. A steam cut-off valve 29 is arranged at the gas inlet of the jacket 201. The water outlet end of the circulating water pipeline 30 is communicated with the water inlet of the jacket 201 of the rectification kettle 2. A circulating water cut-off valve 31 is arranged at the water inlet of the jacket 201. The gas outlet end of the nitrogen pipeline 32 is communicated with the gas inlet of the rectification kettle 2. A nitrogen cut-off valve 33 is arranged at the gas inlet of the rectification kettle 2.

[0039] The signal output ends of the first liquid level sensor 14, the second liquid level sensor 16, the first temperature sensor 15, the second temperature sensor 17 and the pressure sensor 18 are all connected with the signal input end of the controller 34 through signals. The signal output end of the controller 34 is respectively connected with the signal input ends of the transfer pump 12, the feed valve 13, the vacuum unit 10, the reflux ratio regulator 5, the fore-fraction inlet valve 20, the solvent inlet valve 21, the intermediate fraction inlet valve 22, the product inlet valve 23, the fore-fraction gas outlet valve 24, the solvent gas outlet valve 25, the intermediate fraction gas outlet valve 26, the product gas outlet valve 27, the steam cut-off valve 29, the circulating water cut-off valve 31 and the nitrogen cut-off valve 33 through signals.

[0040] The condensation unit 4 includes a water cooler 41 and a salt cooler 42. The gas outlet of the rectification column 3 is communicated with the gas inlet of the water cooler 41. The gas outlet of the water cooler 41 is communicated with the gas inlet of the salt cooler 42. The gas outlet of the salt cooler 42 is communicated with the gas inlet of the vacuum unit 10. The condensate outlets of the water cooler 41 and the salt cooler 42 are both communicated with the liquid inlet of the reflux ratio regulator 5.

[0041] The liquid outlet of the rectifying still 2 is communicated with the feed inlet of the residue storage tank 35 through a discharge pipe 36. A discharge valve 37 and a residue discharge pump 38 are successively arranged on the discharge pipe 36. The signal output end of the controller 34 is signal-connected to the signal input ends of the discharge valve 37 and the residue discharge pump 38 respectively.

[0042] Example 2: A control method for an automated rectification system of triisopropylsilane, which successively includes the following steps:

[0043] (1) Feeding: With one-key start, the transfer pump 12 starts to operate, and at the same time the feed valve 13 opens. 3000 kg of crude product with a purity of 98% enters the rectifying still 2. When the liquid level in the rectifying still 2 reaches the upper limit value or the liquid level in the crude product storage tank 1 reaches the lower limit value, the controller 34 controls the transfer pump 12 and the feed valve 13 to close.

[0044] (2) Receiving the fore fraction: After completing step (1), the controller 34 controls the vacuum unit 10 to start, and at the same time opens the steam cut-off valve 29. When the pressure in the rectifying column 3 < -0.09 MPa, the reflux ratio regulator 5 is controlled to open. All the condensate condensed by the condensation unit 4 flows back into the rectifying column 3, and the reflux time is 1 - 2 h. Then, the controller 34 controls the reflux ratio regulator 5 to adjust the reflux ratio of the condensate flowing back into the rectifying column 3 and the condensate withdrawn into the fore fraction receiving tank 6 to 30:1. At the same time, the fore fraction inlet valve 20 and the fore fraction outlet gas valve 24 are opened. Under the condition that the column diameter and the packing height remain unchanged, by adjusting the reflux ratio, the separation effect is enhanced, and methanol, n-butyl ether, diisopropylsilane, and triisopropylsilane are effectively separated. Under the above reflux ratio conditions, the resolution is relatively high. If the reflux ratio is 40:1, although the resolution is slightly improved, the time required for fore fraction withdrawal is about 7 h, which is too time-consuming and has too high energy consumption.

[0045] (3) Receiving the solvent: When the temperature at the top of the rectifying column 3 in step (2) rises to 80 °C and the difference between the temperature at the top of the rectifying column 3 and the temperature in the rectifying still 2 < 10 °C, the controller 34 controls the fore fraction inlet valve 20 and the fore fraction outlet gas valve 24 to close. At the same time, the solvent inlet valve 21 and the solvent outlet gas valve 25 are opened, and the controller 34 controls the reflux ratio regulator 5 to adjust the reflux ratio of the condensate flowing back into the rectifying column 3 and the condensate withdrawn into the solvent receiving tank 7 to 10:6. At this time, the light components in the fore fraction have been completely separated, and the main fractions are n-butyl ether, diisopropylsilane, and triisopropylsilane. By adjusting the reflux ratio, a large amount of n-butyl ether is withdrawn.

[0046] (4)Receiving of transitional fraction: When the temperature at the top of the rectifying column 3 in step (3) rises to 85 °C, the controller 34 controls the solvent inlet valve 21 and the solvent outlet valve 25 to close, and controls the transitional fraction inlet valve 22 and the transitional fraction outlet valve 26 to open. Meanwhile, the reflux ratio regulator 5 is controlled to adjust the reflux ratio of the condensate refluxed to the rectifying column 3 and the condensate drawn into the transitional fraction tank 8 to be 40:1. The transitional fraction mainly consists of diisopropylsilane and triisopropylsilane. By adjusting a relatively large reflux ratio, diisopropylsilane is separated from the system, thus preparing for the rectification of the product.

[0047] (5)Receiving of product: When the temperature at the top of the rectifying column 3 in step (4) rises to 87 °C, the controller 34 controls the transitional fraction inlet valve 22 and the transitional fraction outlet valve 26 to close, and controls the product inlet valve 23 and the product outlet valve 27 to open. Meanwhile, the reflux ratio regulator 5 is controlled to adjust the reflux ratio of the condensate refluxed to the rectifying column 3 and the condensate drawn into the product receiving tank 9 to be 10:8, effectively drawing out the triisopropylsilane product. After detection, the purity of the triisopropylsilane product reaches over 99.0%, and the yield reaches 80%.

[0048] When the temperature at the top of the rectifying column 3 rises to 90 °C, the controller 34 controls the product inlet valve 23 and the product outlet valve 27 to close. Meanwhile, the reflux ratio regulator 5 is controlled to adjust, and all the condensate is refluxed into the rectifying column 3, and the steam cut-off valve 29 is controlled to close.

[0049] (6)Cooling down: The controller 34 controls the circulating water cut-off valve 31 to open to cool down by introducing cooling water. When the temperature in the rectifying kettle 2 drops below 40 °C, the controller 34 controls the vacuum unit 10 and the reflux ratio regulator 5 to close. After the cooling down is completed, discharging is carried out. The controller 34 controls the nitrogen cut-off valve 33 to open, pressurizes the rectifying kettle 2 to atmospheric pressure and then closes the nitrogen cut-off valve 33. Then the discharging valve 37 is controlled to open, and the kettle residue discharging pump 38 runs to convey the kettle residue in the rectifying kettle 2 into the kettle residue storage tank 35. After the kettle residue in the rectifying kettle 2 is completely discharged, the discharging valve 37 and the kettle residue discharging pump 38 are controlled to close.

[0050] The above is the preferred implementation mode of the present invention. For those of ordinary skill in the art in this technical field, without departing from the principle of the present invention, several improvements and refinements can still be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.

Claims

1. A triisopropylsilane automated distillation control method, characterized in that: It includes the following steps: (1) Feeding: One-button start, the transfer pump starts running, and the feed valve opens at the same time, and the crude product enters the distillation kettle. When the liquid level in the distillation kettle reaches the upper limit, the controller controls the transfer pump and the feed valve to close; (2) Receiving the fore fraction: After completing step (1), the controller controls the vacuum unit to start and opens the steam cut-off valve at the same time. When the pressure in the distillation tower is less than -0.09 MPa, the reflux ratio regulator is controlled to open, and all the condensate condensed by the condensing unit is refluxed into the distillation tower. The reflux time is 1-2 hours. After that, the reflux ratio regulator is controlled to adjust the reflux ratio of the condensate refluxed to the distillation tower and the condensate taken out to the fore fraction receiving tank to 30:

1. At the same time, the fore fraction inlet valve and the fore fraction outlet valve are opened; (3) Solvent receiving: When the temperature of the top of the distillation tower in step (2) rises to 80°C, and the difference between the temperature of the top of the distillation tower and the temperature in the distillation kettle is less than 10°C, the controller controls the front fraction inlet valve and the front fraction outlet valve to be closed, and simultaneously opens the solvent inlet valve and the solvent outlet valve, and controls the reflux ratio regulator to adjust the reflux ratio of the condensate refluxed to the distillation tower and the condensate taken out to the solvent receiving tank to 10:6; (4) Receiving the transition fraction: When the temperature of the top of the distillation tower in step (3) rises to 85° C., the controller controls the solvent inlet valve and the solvent outlet valve to close, and controls the transition fraction inlet valve and the transition fraction outlet valve to open, and at the same time controls the reflux ratio regulator to adjust the reflux ratio of the condensate refluxed to the distillation tower and the condensate taken out to the transition fraction tank to 40:1; (5) Product reception: When the temperature of the top of the distillation tower in step (4) rises to 87°C, the controller controls the transition fraction inlet valve and the transition fraction outlet valve to be closed, and controls the product inlet valve and the product outlet valve to be opened, and controls the reflux ratio regulator to adjust the reflux ratio of the condensate refluxed to the distillation tower and the condensate taken out to the product receiving tank to be 10:8; when the temperature of the top of the distillation tower rises to 90°C, the controller controls the product inlet valve and the product outlet valve to be closed, and controls the reflux ratio regulator to adjust so that all the condensate refluxes into the distillation tower, and controls the steam shut-off valve to be closed; The gas outlet end of the steam pipeline is connected to the gas inlet of the jacket of the distillation kettle; a steam cut-off valve is arranged at the gas inlet of the jacket.

2. The method for controlling the automated distillation of triisopropylsilane according to claim 1, characterized in that: Step (1) also includes that when the liquid level in the crude product storage tank reaches a lower limit value, the controller controls the material transfer pump and the feed valve to close.

3. A triisopropylsilane automated distillation control method according to claim 2, characterized in that: After step (5), the method further includes cooling down: a controller controls the circulating water shut-off valve to open, and cooling water is introduced for cooling down. When the temperature in the distillation kettle drops below 40° C., the controller controls the vacuum unit and the reflux ratio regulator to close.

4. The method for controlling the automated distillation of triisopropylsilane according to claim 3, characterized in that: After cooling is completed, the material is discharged. The controller controls the nitrogen cut-off valve to open, pressurizes the distillation kettle to normal pressure and then closes the nitrogen cut-off valve. Then the discharge valve is controlled to open and the kettle residue discharge pump is operated to transport the kettle residue in the distillation kettle to the kettle residue storage tank. After the kettle residue in the distillation kettle is discharged, the discharge valve and the kettle residue discharge pump are controlled to close.

5. A system for implementing the triisopropylsilane automated distillation control method according to any one of claims 1 to 4, characterized in that: It includes a crude product storage tank, a distillation kettle, a distillation tower, a condensing unit, a reflux ratio regulator, a front fraction receiving tank, a solvent receiving tank, a transition fraction tank, a product receiving tank and a vacuum unit; The liquid outlet of the crude product storage tank is connected to the liquid inlet of the distillation kettle through a feed pipe, and a transfer pump and a feed valve are sequentially arranged on the feed pipe; a first liquid level sensor and a first temperature sensor are arranged in the distillation kettle; The distillation tower is connected to the distillation kettle, the top gas outlet of the distillation tower is connected to the gas inlet of the condensing unit, and the gas outlet of the condensing unit is connected to the gas inlet of the vacuum unit; a second temperature sensor is arranged at the top of the distillation tower; a pressure sensor is arranged in the distillation tower; The condensate outlet of the condensing unit is connected to the liquid inlet of the reflux ratio regulator, and the two liquid outlets of the reflux ratio regulator are respectively connected to the liquid inlet above the distillation tower and the liquid inlet end of the liquid outlet main pipe; The liquid outlet end of the liquid outlet main pipe is respectively connected to the liquid inlets of the fore fraction receiving tank, the solvent receiving tank, the transition fraction tank and the product receiving tank; a fore fraction inlet valve is provided at the liquid inlet of the fore fraction receiving tank; a solvent inlet valve is provided at the liquid inlet of the solvent receiving tank; a transition fraction inlet valve is provided at the liquid inlet of the transition fraction tank; and a product inlet valve is provided at the liquid inlet of the product receiving tank; The top gas outlets of the fore fraction receiving tank, the solvent receiving tank, the transition fraction tank and the product receiving tank are all connected to the gas inlet of the vacuum unit; a fore fraction gas outlet valve is provided at the gas outlet of the fore fraction receiving tank; a solvent gas outlet valve is provided at the gas outlet of the solvent receiving tank; a transition fraction gas outlet valve is provided at the gas outlet of the transition fraction tank; and a product gas outlet valve is provided at the gas outlet of the product receiving tank; The signal output ends of the first liquid level sensor, the first temperature sensor, the second temperature sensor and the pressure sensor are all connected to the signal input end of the controller through signals; the signal output end of the controller is respectively connected to the signal input ends of the material transfer pump, the feed valve, the vacuum unit, the reflux ratio regulator, the front fraction inlet valve, the solvent inlet valve, the transition fraction inlet valve, the product inlet valve, the front fraction outlet valve, the solvent outlet valve, the transition fraction outlet valve, the product outlet valve and the steam cut-off valve through signals.

6. The system according to claim 5, characterized in that The water outlet end of the circulating water pipeline is connected to the water inlet of the jacket of the rectification kettle; a circulating water shut-off valve is arranged at the water inlet of the jacket; The gas outlet end of the nitrogen pipeline is connected to the gas inlet of the distillation kettle, and a nitrogen shut-off valve is arranged at the gas inlet of the distillation kettle; The signal output end of the controller is respectively connected to the signal input ends of the circulating water shut-off valve and the nitrogen shut-off valve through signals.

7. The system according to claim 5, characterized in that A second liquid level sensor is arranged in the crude product storage tank, and a signal output end of the second liquid level sensor is connected to a signal input end of the controller through a signal.

8. The system according to claim 5, characterized in that The vacuum unit is a Roots vacuum unit.

9. The system according to claim 5, characterized in that The condensing unit includes a water cooler and a salt cooler, the air outlet of the distillation tower is connected to the air inlet of the water cooler, the air outlet of the water cooler is connected to the air inlet of the salt cooler, the air outlet of the salt cooler is connected to the air inlet of the vacuum unit, and the condensate outlets of the water cooler and the salt cooler are both connected to the liquid inlet of the reflux ratio regulator.

10. The system according to claim 5, characterized in that It also includes a kettle residue storage tank, the liquid outlet of the distillation kettle is connected to the feed port of the kettle residue storage tank through a discharge pipe, and a discharge valve and a kettle residue discharge pump are sequentially arranged on the discharge pipe; the signal output end of the controller is respectively connected to the signal input end of the discharge valve and the kettle residue discharge pump through signals.

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