Automatic triisopropyl silane rectification system and control method thereof

Abstract

The invention discloses a triisopropyl silane automatic rectification system and a control method thereof, and particularly relates to the technical field of triisopropyl silane extraction, the system comprises a crude product storage tank, a rectification kettle, a rectification tower, a condensation 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 method comprises the following steps: (1) feeding; (2) receiving a front fraction; (3) solvent receiving; (4) receiving a transition fraction; and (5) receiving the product. The triisopropyl silane automatic rectification system and the control method thereof provided by the invention have the beneficial effects that one-key start of the system is realized, the on-site operation state does not need to be operated by personnel, the triisopropyl silane rectification frequency operated by personnel is reduced, and the production cost is reduced; the process operation automation is realized, the continuous and stable execution can be realized, and the qualified triisopropyl silane product is produced.

Description

Technical Field

[0001] The invention relates to the technical field of extracting triisopropylsilane, and specifically to an automated distillation system for triisopropylsilane and a control method thereof. Background Art

[0002] Triisopropylsilane is a chemical intermediate that can be used to synthesize sterically hindered organosilicon protective agents, prepare special organosilicon materials and organic synthesis. It is an excellent hydrogen proton donor and is used in many reduction reactions. The current patent with publication number CN103204869B discloses a method for synthesizing high-purity triisopropylsilane, which discloses the use of magnesium, solvent, 2-chloropropane, methylcyclohexane and trichlorosilane as raw materials for reaction, and then triisopropylsilane is obtained by vacuum distillation; currently, vacuum distillation generally includes crude distillation and rectification, in which rectification is manually controlled, so there is an instability in the control process and large fluctuations, which ultimately affects the output and quality of the product. Summary of the invention

[0003] The object of the present invention is to provide a triisopropylsilane automated distillation system and a control method thereof which realizes process operation automation and reduces production costs.

[0004] The first object of the present invention is implemented by the following technical scheme: an automated distillation system for triisopropylsilane, which comprises 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 gas outlet end of the steam pipeline is connected to the gas inlet of the jacket of the distillation kettle; a steam shut-off valve is provided at the gas inlet of the jacket; 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.

[0005] Furthermore, the water outlet of the circulating water pipeline is connected to the water inlet of the jacket of the distillation kettle; a circulating water shut-off valve is provided 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.

[0006] Furthermore, a second liquid level sensor is provided 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 via a signal.

[0007] Furthermore, the vacuum unit is a Roots vacuum unit.

[0008] Furthermore, 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.

[0009] Furthermore, 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.

[0010] The second objective of the present invention is implemented by the following technical solution: a control method for a triisopropylsilane automated distillation system, comprising 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 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 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 at the same time 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.

[0011] Furthermore, 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.

[0012] Furthermore, after step (5), cooling is also included: the controller controls the circulating water cut-off valve to open, and cooling water is introduced for cooling. When the temperature in the distillation kettle drops below 40° C., the controller controls the vacuum unit and the reflux ratio regulator to close.

[0013] Furthermore, after cooling is completed, the material is discharged, and the controller controls the nitrogen cut-off valve to open, and the nitrogen cut-off valve is closed after the distillation kettle is pressurized to normal pressure. 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 be closed.

[0014] Advantages of the present invention: 1. The present invention provides an automated distillation system for triisopropylsilane, which realizes one-key system startup and does not require human operation during on-site operation, thereby reducing the frequency of human operation for distillation of triisopropylsilane and reducing production costs.

[0015] 2. The present invention provides a control method for an automated distillation system of triisopropylsilane, which performs judgment and control operations based on set process parameters, realizes process operation automation, and can be executed continuously and stably to produce qualified triisopropylsilane products. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0017] Figure 1 This is a process system diagram of Example 1 of the present invention.

[0018] Figure 2 This is a control flow chart of Example 1 of the present invention.

[0019] Crude product storage tank 1, distillation kettle 2, jacket 201, distillation tower 3, condensing unit 4, water cooler 41, salt cooler 42, reflux ratio regulator 5, front fraction receiving tank 6, solvent receiving tank 7, transition 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 total Pipe 19, front fraction inlet valve 20, solvent inlet valve 21, transition fraction inlet valve 22, product inlet valve 23, front fraction outlet valve 24, solvent outlet valve 25, transition fraction outlet valve 26, product 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, kettle residue storage tank 35, discharge pipe 36, discharge valve 37, kettle residue discharge pump 38. DETAILED DESCRIPTION

[0020] The present invention will be further described in detail below by way of examples.

[0021] Example 1: Figure 1 As shown, a triisopropylsilane automated distillation system comprises a crude product storage tank 1, a distillation kettle 2, a distillation tower 3, a condensing unit 4, a reflux ratio regulator 5, a front fraction receiving tank 6, a solvent receiving tank 7, a transition fraction tank 8, a product receiving tank 9, a vacuum unit 10 and a kettle residue storage tank 35; the liquid outlet of the crude product storage tank 1 is connected to the liquid inlet of the distillation 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 distillation valve 13 is arranged in the distillation kettle 2; a first distillation valve 14 is arranged in the distillation kettle 2; a first distillation valve 15 is arranged in the distillation kettle 2; a first distillation valve 16 is arranged in the distillation kettle 2; a first distillation valve 17 is arranged in the distillation kettle 2; a first distillation valve 18 is arranged in the distillation kettle 2; a first distillation valve 19 is arranged in the distillation kettle 2; a first distillation valve 19 is arranged in the distillation kettle 2; a first distillation valve 11 is arranged in the distillation kettle 2; a first distillation valve 12 is arranged in the distillation kettle 2; a first distillation valve 13 is arranged in the distillation kettle 2; a first distillation valve 14 is arranged in the distillation kettle 2; a first distillation valve 15 is arranged in the distillation kettle 2; a first distillation valve 16 is arranged in the distillation kettle 2; a first distillation valve 17 is arranged in the distillation kettle 2; a first distillation valve 18 is arranged in the distillation kettle 2; a first distillation valve 19 is arranged in the distillation kettle 2; a first distillation valve 19 is A liquid level sensor 14 and a first temperature sensor 15; a second liquid level sensor 16 is arranged in the crude product storage tank 1; a distillation tower 3 is arranged above the distillation kettle 2, and the top air outlet of the distillation tower 3 is connected to the air inlet of the condensing unit 4, and the air outlet of the condensing unit 4 is connected to the air 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 of the distillation tower 3; a pressure sensor 18 is arranged in the distillation tower 3.

[0022] The condensate outlet of the condensing unit 4 is connected to the liquid inlet of the reflux ratio regulator 5, and the two liquid outlets of the reflux ratio regulator 5 are respectively connected to the liquid inlet above the distillation tower 3 and the liquid inlet end of the liquid outlet main pipe 19; the liquid outlet end of the liquid outlet main pipe 19 is respectively connected to the liquid inlets of the fore fraction receiving tank 6, the solvent receiving tank 7, the transition fraction tank 8 and the product receiving tank 9; a fore fraction inlet valve 20 is provided at the liquid inlet of the fore fraction receiving tank 6; a solvent inlet valve 21 is provided at the liquid inlet of the solvent receiving tank 7; and a solvent inlet valve 22 is provided at the liquid inlet of the transition fraction tank 8. A transition fraction inlet valve 22; a product inlet valve 23 is provided at the liquid inlet of the product receiving tank 9; the top air outlets of the fore fraction receiving tank 6, the solvent receiving tank 7, the transition fraction tank 8 and the product receiving tank 9 are all connected to the air inlet of the vacuum unit 10; a fore fraction air outlet valve 24 is provided at the air outlet of the fore fraction receiving tank 6; a solvent air outlet valve 25 is provided at the air outlet of the solvent receiving tank 7; a transition fraction air outlet valve 26 is provided at the air outlet of the transition fraction tank 8; and a product air outlet valve 27 is provided at the air outlet of the product receiving tank 9.

[0023] The gas outlet end of the steam pipeline 28 is connected to the gas inlet of the jacket 201 of the distillation kettle 2; a steam shut-off valve 29 is provided at the gas inlet of the jacket 201; the water outlet end of the circulating water pipeline 30 is connected to the water inlet of the jacket 201 of the distillation kettle 2; a circulating water shut-off valve 31 is provided at the water inlet of the jacket 201; the gas outlet end of the nitrogen pipeline 32 is connected to the gas inlet of the distillation kettle 2, and a nitrogen shut-off valve 33 is provided at the gas inlet of the distillation kettle 2.

[0024] 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 to the signal input end of the controller 34 through signals; the signal output end of the controller 34 is respectively connected to the signal input ends of the transfer pump 12, the feed valve 13, the vacuum unit 10, the reflux ratio regulator 5, the front fraction inlet valve 20, the solvent inlet valve 21, the transition fraction inlet valve 22, the product inlet valve 23, the front fraction outlet valve 24, the solvent outlet valve 25, the transition fraction outlet valve 26, the product 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.

[0025] The condensing unit 4 includes a water cooler 41 and a salt cooler 42. The air outlet of the distillation tower 3 is connected to the air inlet of the water cooler 41, the air outlet of the water cooler 41 is connected to the air inlet of the salt cooler 42, the air outlet of the salt cooler 42 is connected to the air inlet of the vacuum unit 10, and the condensate outlets of the water cooler 41 and the salt cooler 42 are both connected to the liquid inlet of the reflux ratio regulator 5.

[0026] The liquid outlet of the distillation kettle 2 is connected to the feed port of the kettle residue storage tank 35 through a discharge pipe 36, on which a discharge valve 37 and a kettle residue discharge pump 38 are sequentially arranged; the signal output end of the controller 34 is respectively connected to the signal input end of the discharge valve 37 and the kettle residue discharge pump 38 through signals.

[0027] Embodiment 2: A control method for a triisopropylsilane automated distillation system, comprising the following steps in sequence: (1) Feeding: One-button start, the transfer pump 12 starts running, and the feed valve 13 opens at the same time, 3000 kg of crude product with a purity of 98% enters the distillation kettle 2. When the liquid level in the distillation kettle 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; (2) Receiving the fore fraction: After completing step (1), the controller 34 controls the vacuum unit 10 to start and opens the steam cut-off valve 29. When the pressure in the distillation tower 3 is less than -0.09 MPa, the reflux ratio regulator 5 is controlled to open, and the condensate condensed by the condensing unit 4 is completely refluxed into the distillation tower 3. The reflux time is 1-2 hours. Then, the reflux ratio regulator 5 is controlled to adjust the reflux ratio of the condensate refluxed to the distillation tower 3 and the condensate taken out 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 valve 24 are opened. When the tower diameter and the packing height remain unchanged, the separation effect is increased by adjusting the reflux ratio, and methanol, n-butyl ether, diisopropylsilane and triisopropylsilane are effectively separated. Under the above reflux ratio conditions, the separation degree is relatively high. If the reflux ratio is 40:1, although the separation degree is slightly improved, the fore fraction takes about 7 hours to be taken out, which is too long and the energy consumption is too high.

[0028] (3) Solvent receiving: When the temperature at the top of the distillation tower 3 in step (2) is raised to 80°C, and the difference between the temperature at the top of the distillation tower 3 and the temperature in the distillation kettle 2 is less than 10°C, the controller 34 controls the front fraction inlet valve 20 and the front fraction outlet valve 24 to be closed, and simultaneously opens the solvent inlet valve 21 and the solvent outlet valve 25, and controls the reflux ratio regulator 5 to adjust the reflux ratio of the condensate refluxed to the distillation tower 3 and the condensate taken out to the solvent receiving tank 7 to 10:6; at this time, the light components in the front fraction have been separated, and the main fractions are n-butyl ether, diisopropyl silane and triisopropyl silane. The reflux ratio is adjusted to take out a large amount of n-butyl ether.

[0029] (4) Receiving the transition fraction: When the temperature at the top of the distillation tower 3 in step (3) rises to 85° C., the controller 34 controls the solvent inlet valve 21 and the solvent outlet valve 25 to be closed, and controls the transition fraction inlet valve 22 and the transition fraction outlet valve 26 to be opened. At the same time, the reflux ratio regulator 5 is controlled to adjust the reflux ratio of the condensate refluxed to the distillation tower 3 and taken out to the transition fraction tank 8 to 40:1; the transition fraction is mainly diisopropylsilane and triisopropylsilane. A larger reflux ratio is adjusted to separate diisopropylsilane from the system, thereby preparing for product distillation.

[0030] (5) Product reception: When the temperature at the top of the distillation tower 3 in step (4) rises to 87° C., the controller 34 controls the transition fraction inlet valve 22 and the transition fraction outlet valve 26 to be closed, and controls the product inlet valve 23 and the product outlet valve 27 to be opened. At the same time, the reflux ratio regulator 5 is controlled to adjust the reflux ratio of the condensate refluxed to the distillation tower 3 and the condensate produced into the product receiving tank 9 to 10:8, thereby effectively producing the triisopropylsilane product. The purity of the triisopropylsilane product is found to be above 99.0%, and the yield is found to be 80%.

[0031] When the top of the distillation tower 3 is heated to 90°C, the controller 34 controls the product inlet valve 23 and the product outlet valve 27 to close, and at the same time controls the reflux ratio regulator 5 to adjust so that all the condensate flows back into the distillation tower 3, and controls the steam shut-off valve 29 to close.

[0032] (6) Cooling: The controller 34 controls the circulating water shut-off valve 31 to open and introduces cooling water for cooling. When the temperature in the distillation kettle 2 drops to below 40°C, the controller 34 controls the vacuum unit 10 and the reflux ratio regulator 5 to close. After the cooling is completed, the material is discharged. The controller 34 controls the nitrogen shut-off valve 33 to open, pressurizes the distillation kettle 2 to normal pressure, and then closes the nitrogen shut-off valve 33. Then, the discharge valve 37 is controlled to open, and the kettle residue discharge pump 38 is operated to transport the kettle residue in the distillation kettle 2 to the kettle residue storage tank 35. After the kettle residue in the distillation kettle 2 is discharged, the discharge valve 37 and the kettle residue discharge pump 38 are controlled to close.

[0033] The above are preferred embodiments of the present invention. For ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.

Claims

1. A triisopropylsilane automated distillation system, 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 gas outlet end of the steam pipeline is connected to the gas inlet of the jacket of the distillation kettle; a steam shut-off valve is provided at the gas inlet of the jacket; 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.

2. The triisopropylsilane automated distillation system according to claim 1, 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.

3. The triisopropylsilane automated distillation system according to claim 1, 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.

4. The triisopropylsilane automated distillation system according to claim 1, characterized in that: The vacuum unit is a Roots vacuum unit.

5. The triisopropylsilane automated distillation system according to claim 1, 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.

6. The triisopropylsilane automated distillation system according to claim 1, 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.

7. A control method for a system as claimed in any one of claims 1 to 6, 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 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 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 at the same time 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.

8. The control method of a triisopropylsilane automated distillation system according to claim 7, 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.

9. The control method of a triisopropylsilane automated distillation system according to claim 7, 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.

10. The control method of a triisopropylsilane automated distillation system according to claim 9, 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.

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