Comprehensive utilization system for slag discharged by cold hydrogenation

By designing a comprehensive utilization system for cold hydrogenated discharge slag materials, efficient separation and recovery of valuable components in the slag materials are achieved, and the problem of underutilization of slag materials is solved, especially the high-purity recovery of hexachlorodisilane and the environmentally friendly treatment of solid phase materials.

CN223287751UActive Publication Date: 2025-09-02SICHUAN YONGXIANG CO LTD
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Patent Information

Application Number
CN202422249597.5
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-09-13
Publication Date
2025-09-02
Estimated Expiration
2034-09-13

AI Technical Summary

Technical Problem

During the existing polysilicon production process, the slag material emitted by cold hydrogenation contains a large amount of by-products and is not fully utilized, especially the slag material emitted by the scrubber in the trichlorosilicon production process contains metal chloride, microsilicon powder, etc., which cannot be effectively recycled and utilized.

Method used

A comprehensive utilization system for slag material discharged by cold hydrogenation is designed. Through the combination of settling tank, distillation tower and distillation tower, multiple distillation of slag material is realized, high-purity hexachlorodiosilane is separated, and solid phase metal chloride and silicon powder are sent to the hydrolysis tank for hydrolysis treatment.

Benefits of technology

It realizes efficient recycling of valuable components in the slag material, especially the purity of hexachlorodisilane reaches 99.9%, and converts solid phase materials into silicon oxide and hydrogen chloride to meet environmental protection treatment requirements.

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Abstract

The utility model discloses a comprehensive utilization system for slag discharged by cold hydrogenation, which belongs to the technical field of polycrystalline silicon production and is characterized in that the slag discharged by cold hydrogenation is in a settling tank, supernatant liquid is filtered by a filter and then enters a distillation tower to be distilled, and partial distilled fraction enters a first rectifying tower to be rectified for the first time; the tower kettle produced liquid of the first rectifying tower enters a second rectifying tower (the middle upper part of the second rectifying tower is fed) for secondary rectification, and the tower top produced liquid of the second rectifying tower is discharged through a product outlet pipe to obtain high-purity hexachlorodisilane.
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Description

Technical Field

[0001] The utility model belongs to the technical field of polysilicon production, and in particular relates to a comprehensive utilization system for slag discharged from cold hydrogenation. Background Art

[0002] Currently, polysilicon is primarily produced using the trichlorosilane reduction method and the silane fluidized bed method. Both methods use industrial silicon powder, H₂, hydrogen chloride, and silicon tetrachloride as raw materials to produce trichlorosilane. The silicon powder undergoes a chemical reaction in the presence of a catalyst within a hydrogenation furnace to produce trichlorosilane. In addition to monosilicon-containing chlorosilane, this process also produces small amounts of disilicon- or polysilicon-containing chlorosilane byproducts. These byproducts are primarily removed through hydrolysis or cracked into trichlorosilane feedstock, and their value is not fully realized.

[0003] The slag discharged from the washing tower in the trichlorosilane (cold hydrogenation) production process is mainly composed of metal (magnesium, aluminum, iron, calcium, etc.) chlorides, trace amounts of microsilica, hexachlorodisilane, hexachlorodisiloxane, silicon tetrachloride, a small amount of trichlorosilane, a very small amount of methylchlorosilanes, dimethylchlorosilanes, ethylchlorosilanes, polymethylsilane, silicone oil, etc., as well as very small amounts of dissolved gases such as HCl, H2, N2, etc. Utility Model Content

[0004] In order to solve the above technical problems, the utility model provides a comprehensive utilization system for slag discharged from cold hydrogenation. The slag discharged from cold hydrogenation is placed in a settling tank, and the supernatant liquid is filtered through a filter and then enters a distillation tower for distillation. Part of the distilled fraction enters a first distillation tower (feeding the lower part of the first distillation tower) for the first distillation, and the produced liquid from the kettle of the first distillation tower enters a second distillation tower (feeding the upper part of the second distillation tower) for the second distillation. The produced liquid from the top of the second distillation tower is discharged through a product outlet pipe to obtain high-purity hexachlorodisilane.

[0005] The purpose of this utility model is achieved through the following technical solutions:

[0006] A comprehensive utilization system for slag discharged from cold hydrogenation comprises a settling tank, wherein a feed pipe and a supernatant outlet pipe are provided on the settling tank, the supernatant outlet pipe is connected to a distillation tower via a filter, a distillation outlet pipe is provided on the distillation tower, a first condenser is provided on the distillation outlet pipe, the distillation outlet pipe is connected to a first fractionation pipe and a second fractionation pipe, the first fractionation pipe is provided with a first fractionation tank and a first efflux pump, the second fractionation pipe is connected to a first rectifying tower, the first rectifying tower is provided with a first reflux assembly and a first liquid outlet pipe, the first reflux assembly is connected to a chlorosilane discharge pipe, the first liquid outlet pipe is connected to a second rectifying tower, the second reflux assembly is provided on the second rectifying tower and is connected to the second liquid outlet pipe, and the second reflux assembly is connected to a product outlet pipe.

[0007] Preferably, the distillation tower is provided with a first temperature control unit; and the first fractionation tank is provided with a first pressure control unit.

[0008] Preferably, the first pressure control unit includes a first pressure sensor, a first tail gas control valve, a distillate outlet pipe, a distillate pipe and a heat exchanger, the first pressure sensor is arranged on the distillation tower, the first fractionation tank is connected to the heat exchanger through the distillate outlet pipe, the heat exchanger is connected to the first fractionation tank through the distillate pipe, the heat exchanger is provided with a first tail gas outlet pipe, and the first tail gas control valve is provided on the first tail gas outlet pipe.

[0009] Preferably, the first temperature control unit includes a first temperature sensor, a first fractionation control valve and a second fractionation control valve, and the first fractionation control valve and the second fractionation control valve are respectively arranged on the first fractionation pipe and the second fractionation pipe.

[0010] Preferably, the first reflux assembly includes a first distillation outlet pipe, a first reflux tank, a first reflux pump and a first reflux pipe, a second condenser is provided on the first distillation outlet pipe, the first distillation tower is connected to the first reflux tank through the first distillation outlet pipe, the first reflux tank is connected to the first distillation tower through the first reflux pump and the first reflux pipe, and the first reflux pipe is connected to the chlorosilane discharge pipe.

[0011] Preferably, a second pressure control unit is provided on the first reflux tank, and the second pressure control unit includes a second pressure sensor, a second tail gas pipe and a second tail gas control valve. The second tail gas pipe is connected to the first reflux tank, the second pressure sensor is provided on the first reflux tank, and the second tail gas control valve is provided on the second tail gas pipe.

[0012] Preferably, the second reflux assembly includes a second distillation outlet pipe, a second reflux tank, a second reflux pump and a second reflux pipe, a third condenser is provided on the second distillation outlet pipe, the second distillation tower is connected to the second reflux tank through the second distillation outlet pipe, the second reflux tank is connected to the second distillation tower through the second reflux pump and the second reflux pipe, and the second reflux pipe is connected to the product outlet pipe.

[0013] Preferably, a third pressure control unit is provided on the second reflux tank, and the third pressure control unit includes a third pressure sensor, a third tail gas pipe and a third tail gas control valve. The third tail gas pipe is connected to the second reflux tank, the third pressure sensor is provided on the second reflux tank, and the third tail gas control valve is provided on the third tail gas pipe.

[0014] Preferably, a first slag discharge pipe is provided at the lower end of the sedimentation tank, and a second slag discharge pipe is provided at the lower end of the distillation tower. The first slag discharge pipe and the second slag discharge pipe are connected to the waste liquid tank. A third slag discharge pipe is provided at the lower end of the waste liquid tank, and the third slag discharge pipe is connected to the hydrolysis tank. A water inlet pipe and a fourth slag discharge pipe are provided on the hydrolysis tank, and the fourth slag discharge pipe is connected to the wastewater treatment unit through a wastewater pump.

[0015] Preferably, the sedimentation tank, waste liquid tank and hydrolysis tank are respectively provided with a fourth pressure control unit, a fifth pressure control unit and a second temperature control unit; the fourth pressure control unit includes a fourth pressure sensor, a fourth tail gas outlet pipe and a fourth vent valve, the fourth pressure sensor and the fourth tail gas outlet pipe are both provided on the sedimentation tank, and the fourth vent valve is provided on the fourth tail gas outlet pipe; the fifth pressure control unit includes a fifth pressure sensor, a fifth tail gas outlet pipe and a fifth vent valve, the fifth pressure sensor and the fifth tail gas outlet pipe are both provided on the waste liquid tank, and the fifth vent valve is provided on the fifth tail gas outlet pipe; the second temperature control unit includes a second temperature sensor, a water inlet pipe and a water supply valve, the second temperature sensor and the water inlet pipe are provided on the hydrolysis tank, and the water supply valve is provided on the water inlet pipe.

[0016] Preferably, the first liquid outlet pipe and the second liquid outlet pipe are respectively provided with a first tower bottom pump and a second tower bottom pump.

[0017] The beneficial effects of this technical solution are as follows:

[0018] 1. The utility model provides a comprehensive utilization system for slag discharged from cold hydrogenation. The slag discharged from cold hydrogenation is placed in a settling tank. The supernatant liquid is filtered through a filter and then enters a distillation tower for distillation. Part of the distilled fraction enters a first distillation tower for a first distillation. The produced liquid from the kettle of the first distillation tower enters a second distillation tower (feeding the upper part of the second distillation tower) for a second distillation. The produced liquid from the top of the second distillation tower is discharged through a product outlet pipe to obtain high-purity hexachlorodisilane.

[0019] 2. The utility model provides a comprehensive utilization system for slag discharged from cold hydrogenation. The slag discharged from cold hydrogenation is settled in a settling tank (solid metal chlorides, fine silicon powder and other solid particles are precipitated at the bottom of the settling tank during settling and discharged regularly). The supernatant is filtered through a filter and then enters a distillation tower. When the temperature of the distillation tower is less than 80°C, it switches to a first distillation tank, and when the temperature is ≥80°C, it switches to a second distillation tank. The material in the second distillation tank is sent to a first distillation tower (feeding the lower part of the first distillation tower) for a first distillation (the first distillation removes components in the second distillation with a boiling point lower than hexachlorodisilane from the top of the tower). The produced liquid from the bottom of the first distillation tower is sent to a second distillation tower (feeding the upper part of the second distillation tower) for a second distillation (the second distillation removes materials with a boiling point higher than hexachlorodisilane from the bottom of the tower). The produced liquid from the top of the second distillation tower is discharged through a product outlet pipe to obtain high-purity hexachlorodisilane.

[0020] The present invention provides a comprehensive utilization system for cold hydrogenation slag. The distillation tower bottom material and the lower sediment in the settling tank are discharged into a waste liquid tank, which serves as a hydrolysis buffer tank. Solid metal chlorides and silicon powder are carried from the bottom of the settling tank into the waste liquid tank by gravity and pressure differentials, driven by the flow of the liquid phase. In the hydrolysis tank, a large amount of water reacts with the materials in the settling tank, hydrolyzing the silicon-containing materials into silicon oxide and hydrogen chloride. These, along with the silicon powder, metal chlorides, and other materials, are then sent to the environmental protection process for wastewater treatment. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is a structural diagram of the utility model;

[0022] In the figure: 1, settling tank; 2, feed pipe; 3, supernatant outlet pipe; 4, filter; 5, distillation tower; 6, distillation outlet pipe; 7, first condenser; 8, first fractionating pipe; 9, second fractionating pipe; 10, first fractionating tank; 11, first efflux pump; 12, first rectification tower; 13, first reflux assembly; 131, first rectification outlet pipe; 132, first reflux tank; 133, first reflux pump; 134, first reflux pipe; 135, second condenser; 14, first liquid outlet pipe; 15, chlorosilane outlet pipe; 16, second distillation tower; 17, second reflux assembly; 171, second distillation outlet pipe; 172, second reflux tank; 173, second reflux pump; 174, second reflux pipe; 175, third condenser; 18, second liquid outlet pipe; 19, product outlet pipe; 20, first temperature control unit; 201, first temperature sensor; 202, first fractionation control valve; 203, second fractionation control valve; 21, first pressure control unit; 211, first pressure sensor; 212, first tail gas control valve ; 213, distillate outlet pipe; 214, distillate pipe; 215, heat exchanger; 216, first tail gas outlet pipe; 22, second pressure control unit; 221, second pressure sensor; 222, second tail gas pipe; 223, second tail gas control valve; 23, third pressure control unit; 231, third pressure sensor; 232, third tail gas pipe; 233, third tail gas control valve; 24, first slag discharge pipe; 25, second slag discharge pipe; 26, waste liquid tank; 27, third slag discharge pipe; 28, hydrolysis tank; 2 9. Water inlet pipe; 30. Fourth slag discharge pipe; 31. Wastewater pump; 32. Wastewater treatment unit; 33. First tower bottom pump; 34. Second tower bottom pump; 35. Fourth pressure control unit; 351. Fourth pressure sensor; 352. Fourth tail gas outlet pipe; 353. Fourth vent valve; 36. Fifth pressure control unit; 361. Fifth pressure sensor; 362. Fifth tail gas outlet pipe; 363. Fifth vent valve; 37. Second temperature control unit; 371. Second temperature sensor; 372. Water supply valve. DETAILED DESCRIPTION

[0023] The present invention will be further described in detail below with reference to the embodiments, but the embodiments of the present invention are not limited thereto.

[0024] Example 1

[0025] like Figure 1As shown, a comprehensive utilization system for slag discharged from cold hydrogenation includes a settling tank 1, a feed pipe 2 and a supernatant outlet pipe 3 are provided on the settling tank 1, the supernatant outlet pipe 3 is connected to a distillation tower 5 through a filter 4, a distillation outlet pipe 6 is provided on the distillation tower 5, a first condenser 7 is provided on the distillation outlet pipe 6, the distillation outlet pipe 6 is connected to a first fractionation pipe 8 and a second fractionation pipe 9, the first fractionation pipe 8 is provided with a first fractionation tank 10 and a first efflux pump 11, the second fractionation pipe 9 is connected to a first rectifying tower 12, the first rectifying tower 12 is provided with a first reflux assembly 13 and a first liquid outlet pipe 14, the first reflux assembly 13 is connected to a chlorosilane discharge pipe 15, the first liquid outlet pipe 14 is connected to a second rectifying tower 16, the second rectifying tower 16 is provided with a second reflux assembly 17 and a second liquid outlet pipe 18, and the second reflux assembly 17 is connected to a product outlet pipe 19. The filter 4 is used as one and is for backup, and the filter screen adopts a 40-100 mesh filter screen.

[0026] Example 2

[0027] The difference between this embodiment and embodiment 1 is that the distillation tower 5 is provided with a first temperature control unit 20 ; and the first fractionation tank 10 is provided with a first pressure control unit 21 .

[0028] The first pressure control unit 21 includes a first pressure sensor 211, a first tail gas control valve 212, a fraction outlet pipe 213, a fraction pipe 214, and a heat exchanger 215. The first pressure sensor 211 is mounted on the distillation tower 5. The first fractionating tank 10 is connected to the heat exchanger 215 via the fraction outlet pipe 213. The heat exchanger 215 is connected to the first fractionating tank 10 via the fraction pipe 214. The heat exchanger 215 is mounted on a first tail gas outlet pipe 216. The first tail gas control valve 212 is mounted on the first tail gas outlet pipe 216. The first pressure sensor 211 detects the pressure within the distillation tower 5 and transmits the pressure signal to the DCS, which controls the opening or closing of the first tail gas control valve 212.

[0029] The first temperature control unit 20 includes a first temperature sensor 201, a first fractionation control valve 202, and a second fractionation control valve 203. The first fractionation control valve 202 and the second fractionation control valve 203 are respectively disposed on the first fractionation pipe 8 and the second fractionation pipe 9. The first temperature sensor 201 detects the temperature within the distillation column 5 and transmits the temperature signal to the DCS, which controls the opening or closing of the first fractionation control valve 202 and the second fractionation control valve 203.

[0030] Among them, the first reflux component 13 includes a first distillation outlet pipe 131, a first reflux tank 132, a first reflux pump 133 and a first reflux pipe 134, the first distillation outlet pipe 131 is provided with a second condenser 135, the first distillation tower 12 is connected to the first reflux tank 132 through the first distillation outlet pipe 131, the first reflux tank 132 is connected to the first distillation tower 12 through the first reflux pump 133 and the first reflux pipe 134, and the first reflux pipe 134 is connected to the chlorosilane discharge pipe 15.

[0031] The first reflux tank 132 is provided with a second pressure control unit 22, which includes a second pressure sensor 221, a second tail gas pipe 222, and a second tail gas control valve 223. The second tail gas pipe 222 is connected to the first reflux tank 132, the second pressure sensor 221 is provided on the first reflux tank 132, and the second tail gas control valve 223 is provided on the second tail gas pipe 222. The second pressure sensor 221 detects the pressure in the first reflux tank 132 and transmits the pressure signal to the DCS, which controls the opening or closing of the second tail gas control valve 223.

[0032] Among them, the second reflux component 17 includes a second distillation outlet pipe 171, a second reflux tank 172, a second reflux pump 173 and a second reflux pipe 174, the second distillation outlet pipe 171 is provided with a third condenser 175, the second distillation tower 16 is connected to the second reflux tank 172 through the second distillation outlet pipe 171, the second reflux tank 172 is connected to the second distillation tower 16 through the second reflux pump 173 and the second reflux pipe 174, and the second reflux pipe 174 is connected to the product outlet pipe 19.

[0033] The second reflux tank 172 is provided with a third pressure control unit 23, which includes a third pressure sensor 231, a third tail gas pipe 232, and a third tail gas control valve 233. The third tail gas pipe 232 is connected to the second reflux tank 172, the third pressure sensor 231 is provided on the second reflux tank 172, and the third tail gas control valve 233 is provided on the third tail gas pipe 232. The third pressure sensor 231 detects the pressure in the second reflux tank 172 and transmits the pressure signal to the DCS, which controls the opening or closing of the third tail gas control valve 233.

[0034] Among them, a first slag discharge pipe 24 is provided at the lower end of the sedimentation tank 1, and a second slag discharge pipe 25 is provided at the lower end of the distillation tower 5. The first slag discharge pipe 24 and the second slag discharge pipe 25 are connected to the waste liquid tank 26. A third slag discharge pipe 27 is provided at the lower end of the waste liquid tank 26. The third slag discharge pipe 27 is connected to the hydrolysis tank 28. The hydrolysis tank 28 is provided with a water inlet pipe 29 and a fourth slag discharge pipe 30. The fourth slag discharge pipe 30 is connected to the wastewater treatment unit 32 through a wastewater pump 31.

[0035] The sedimentation tank 1, the waste liquid tank 26 and the hydrolysis tank 28 are respectively provided with a fourth pressure control unit 35, a fifth pressure control unit 36 ​​and a second temperature control unit 37; the fourth pressure control unit 35 includes a fourth pressure sensor 351, a fourth tail gas outlet pipe 352 and a fourth vent valve 353, the fourth pressure sensor 351 and the fourth tail gas outlet pipe 352 are both provided on the sedimentation tank 1, and the fourth vent valve 353 is provided on the fourth tail gas outlet pipe 352; the fifth pressure control unit 35 includes a fourth pressure sensor 351, a fourth tail gas outlet pipe 352 and a fourth vent valve 353, the fourth pressure sensor 351 and the fourth tail gas outlet pipe 352 are both provided on the sedimentation tank 1, and the fourth vent valve 353 is provided on the fourth tail gas outlet pipe 352; 6 includes a fifth pressure sensor 361, a fifth tail gas outlet pipe 362, and a fifth vent valve 363. The fifth pressure sensor 361 and the fifth tail gas outlet pipe 362 are both located on the waste liquid tank 26, and the fifth vent valve 363 is located on the fifth tail gas outlet pipe 362. The second temperature control unit 37 includes a second temperature sensor 371, a water inlet pipe 29, and a water replenishment valve 373. The second temperature sensor 371 and the water inlet pipe 29 are located on the hydrolysis tank 28, and the water replenishment valve 373 is located on the water inlet pipe 29. The fourth pressure sensor 351, the fifth pressure sensor 361, and the second temperature sensor 371 respectively detect the pressure of the sedimentation tank 1, the pressure of the waste liquid tank 26, and the temperature of the hydrolysis tank 28. The pressure signals of the sedimentation tank 1, the pressure signals of the waste liquid tank 26, and the temperature signals of the hydrolysis tank 28 are transmitted to the DCS, which controls the opening or closing of the fourth vent valve 353, the fifth vent valve 363, and the water replenishment valve 373.

[0036] The first liquid outlet pipe 14 and the second liquid outlet pipe 18 are respectively provided with a first tower bottom pump 33 and a second tower bottom pump 34 .

[0037] Using the above system, a method for comprehensive utilization of slag discharged from cold hydrogenation comprises the following steps:

[0038] Step 1, cold hydrogenation production process: The slag discharged from the washing tower enters the settling tank 1 through the feed pipe 2, the slag is deposited in the settling tank 1, and the supernatant passes through the supernatant outlet pipe 3 and is filtered by the filter 4 before entering the distillation tower 5; the temperature of the material in the feed pipe 2 is controlled at 40-50°C; the pressure in the settling tank 1 is controlled at 20-30kPa; and the tower pressure in the distillation tower 5 is controlled at 40-50kPa;

[0039] Step 2: The supernatant liquid is distilled in the distillation tower 5. The first temperature control unit 20 and the first pressure control unit 21 on the distillation tower 5 are started, and the temperature of the first condenser 7 is controlled to be less than or equal to 50°C. When the temperature on the distillation tower 5 is greater than or equal to 80°C and less than or equal to 160°C, the first fractionation control valve 202 is closed, the second fractionation control valve 203 is opened, and the distillate flows into the first rectifying tower 12 through the second fractionation pipe 9. When the temperature on the distillation tower 5 is greater than 160°C, both the first fractionation control valve 202 and the second fractionation control valve are closed, and the distillate from the distillation tower 5 is discharged through the second slag discharge pipe 25.

[0040] Step 3: The distillate is subjected to a primary distillation in the first distillation tower 12. The overhead distillate of the first distillation tower 12 is partially refluxed to the first distillation tower 12 through the first reflux assembly 13, and partially flows into the chlorosilane raw material tank through the chlorosilane discharge pipe 15. The effluent from the bottom of the first distillation tower 12 flows into the second distillation tower 16 through the first liquid outlet pipe 14.

[0041] Step 4: The effluent from the bottom of the first distillation tower 12 is subjected to secondary distillation in the second distillation tower 16. The top distillate of the second distillation tower 16 is partially refluxed to the second distillation tower 16 through the second reflux component 17, and partially flows out through the product outlet pipe 19; the effluent from the bottom of the second distillation tower 16 flows into the settling tank 1 through the second liquid outlet pipe 18.

[0042] Among them, it also includes the start-up of the first pressure control unit 21, the second pressure control unit 22 and the third pressure control unit 23; when the pressure of the first distillation tank 10 exceeds 50kpa, the first tail gas control valve 212 is opened to discharge the tail gas from the first tail gas outlet pipe 216; when the pressure of the first reflux tank 132 exceeds 150kpa, the second tail gas control valve 223 is opened to discharge the tail gas from the second tail gas pipe 222; when the pressure of the second reflux tank 172 exceeds 150kpa, the third tail gas control valve 233 is opened to discharge the tail gas from the third tail gas pipe 232.

[0043] The process also includes starting the fourth pressure control unit 35, the fifth pressure control unit 36 ​​and the second temperature control unit 37; the contents of the distillation tower 5 and the lower sediment in the sedimentation tank 1 are discharged into the waste liquid tank 26, which collects the contents while stirring. After collecting the contents, the waste liquid tank 26 discharges the contents into the hydrolysis tank 28 through the third slag discharge pipe 27; industrial water is added to the hydrolysis tank 28 through the water inlet pipe 29, and after hydrolysis in the hydrolysis tank 28, it is transported to the waste water treatment unit 32 through the fourth slag discharge pipe 30 and the waste water pump 31; the tower pressure of the first distillation tower 12 is controlled at 110-120 kPa, and the tower temperature is controlled at 80 The temperature is -192°C, the theoretical plate is 180, and the reflux ratio of the first reflux assembly 13 is 3. The effluent from the bottom of the first distillation tower 12 flows into the second distillation tower 16 through the first liquid outlet pipe 14 for a second distillation. The tower pressure of the second distillation tower 16 is controlled at 110-120 kPa, the tower temperature is controlled at 172-192°C, the theoretical plate is 150, and the reflux ratio of the second reflux assembly 17 is 9. The overhead distillate of the second distillation tower 16 is partially refluxed to the second distillation tower 16 through the second reflux assembly 17, and partially flows out through the product outlet pipe 19. The purity of hexachlorodisilane in the product is greater than 99.9% (better than the purity requirements of GB / T 42720-2023 "Electronic Special Gas Hexachlorodisiloxane"), and contains trace amounts of hexachlorodisiloxane at the ppm level and silicone oil impurities at the ppt level.

[0044] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Any simple modification or equivalent change made to the above embodiment based on the technical essence of the present invention falls within the scope of protection of the present invention.

Claims

1. A comprehensive utilization system for slag discharged from cold hydrogenation, characterized by: The invention comprises a settling tank (1), wherein a feed pipe (2) and a supernatant outlet pipe (3) are provided on the settling tank (1), wherein the supernatant outlet pipe (3) is connected to a distillation tower (5) through a filter (4), wherein a distillation outlet pipe (6) is provided on the distillation tower (5), wherein a first condenser (7) is provided on the distillation outlet pipe (6), wherein the distillation outlet pipe (6) is connected to a first fractionation pipe (8) and a second fractionation pipe (9), wherein a first fractionation tank (10) and a first efflux pump (11) are provided on the first fractionation pipe (8), wherein the first fractionation pipe (8) is provided with a first fractionation tank (10) and a first efflux pump (1 ... The second fractionating pipe (9) is connected to the first distillation tower (12); the first distillation tower (12) is provided with a first reflux component (13) and a first liquid outlet pipe (14); the first reflux component (13) is connected to the chlorosilane outlet pipe (15); the first liquid outlet pipe (14) is connected to the second distillation tower (16); the second distillation tower (16) is provided with a second reflux component (17) connected to the second liquid outlet pipe (18); the second reflux component (17) is connected to the product outlet pipe (19).

2. The comprehensive utilization system for slag discharged from cold hydrogenation according to claim 1, characterized in that: The distillation tower (5) is provided with a first temperature control unit (20); and the first fractionation tank (10) is provided with a first pressure control unit (21).

3. The comprehensive utilization system for slag discharged from cold hydrogenation according to claim 2, characterized in that: The first pressure control unit (21) comprises a first pressure sensor (211), a first tail gas control valve (212), a fraction outlet pipe (213), a fraction pipe (214), and a heat exchanger (215); the first pressure sensor (211) is arranged on the distillation tower (5); the first fractionating tank (10) is connected to the heat exchanger (215) via the fraction outlet pipe (213); the heat exchanger (215) is connected to the first fractionating tank (10) via the fraction pipe (214); the heat exchanger (215) is provided with a first tail gas outlet pipe (216); and the first tail gas control valve (212) is arranged on the first tail gas outlet pipe (216).

4. The comprehensive utilization system for slag discharged from cold hydrogenation according to claim 3, characterized in that: The first temperature control unit (20) comprises a first temperature sensor (201), a first fractionation control valve (202) and a second fractionation control valve (203), wherein the first fractionation control valve (202) and the second fractionation control valve (203) are respectively arranged on the first fractionation pipe (8) and the second fractionation pipe (9).

5. The comprehensive utilization system for slag discharged from cold hydrogenation according to claim 4, characterized in that: The first reflux assembly (13) comprises a first distillation outlet pipe (131), a first reflux tank (132), a first reflux pump (133) and a first reflux pipe (134); a second condenser (135) is provided on the first distillation outlet pipe (131); the first distillation tower (12) is connected to the first reflux tank (132) via the first distillation outlet pipe (131); the first reflux tank (132) is connected to the first distillation tower (12) via the first reflux pump (133) and the first reflux pipe (134); and the first reflux pipe (134) is connected to the chlorosilane discharge pipe (15).

6. The comprehensive utilization system for slag discharged from cold hydrogenation according to claim 5, characterized in that: A second pressure control unit (22) is provided on the first reflux tank (132), the second pressure control unit (22) comprising a second pressure sensor (221), a second tail gas pipe (222) and a second tail gas control valve (223), the second tail gas pipe (222) being connected to the first reflux tank (132), the second pressure sensor (221) being provided on the first reflux tank (132), and the second tail gas control valve (223) being provided on the second tail gas pipe (222).

7. The comprehensive utilization system for slag discharged from cold hydrogenation according to claim 6, characterized in that: The second reflux assembly (17) includes a second distillation outlet pipe (171), a second reflux tank (172), a second reflux pump (173) and a second reflux pipe (174); a third condenser (175) is provided on the second distillation outlet pipe (171); the second distillation tower (16) is connected to the second reflux tank (172) via the second distillation outlet pipe (171); the second reflux tank (172) is connected to the second distillation tower (16) via the second reflux pump (173) and the second reflux pipe (174); and the second reflux pipe (174) is connected to the product outlet pipe (19).

8. The comprehensive utilization system for slag discharged from cold hydrogenation according to claim 7, characterized in that: A third pressure control unit (23) is provided on the second reflux tank (172), the third pressure control unit (23) comprising a third pressure sensor (231), a third tail gas pipe (232) and a third tail gas control valve (233), the third tail gas pipe (232) being connected to the second reflux tank (172), the third pressure sensor (231) being provided on the second reflux tank (172), and the third tail gas control valve (233) being provided on the third tail gas pipe (232).

9. The comprehensive utilization system for slag discharged from cold hydrogenation according to claim 8, characterized in that: A first slag discharge pipe (24) is provided at the lower end of the settling tank (1), and a second slag discharge pipe (25) is provided at the lower end of the distillation tower (5). The first slag discharge pipe (24) and the second slag discharge pipe (25) are connected to a waste liquid tank (26). A third slag discharge pipe (27) is provided at the lower end of the waste liquid tank (26). The third slag discharge pipe (27) is connected to a hydrolysis tank (28). A water inlet pipe (29) and a fourth slag discharge pipe (30) are provided on the hydrolysis tank (28). The fourth slag discharge pipe (30) is connected to a wastewater treatment unit (32) via a wastewater pump (31).

10. The comprehensive utilization system for slag discharged from cold hydrogenation according to claim 9, characterized in that: The sedimentation tank (1), the waste liquid tank (26) and the hydrolysis tank (28) are respectively provided with a fourth pressure control unit (35), a fifth pressure control unit (36) and a second temperature control unit (37); the fourth pressure control unit (35) comprises a fourth pressure sensor (351), a fourth tail gas outlet pipe (352) and a fourth vent valve (353); the fourth pressure sensor (351) and the fourth tail gas outlet pipe (352) are both provided on the sedimentation tank (1), and the fourth vent valve (353) is provided on the fourth tail gas outlet pipe (352); the fifth pressure control unit (351) comprises a fourth pressure sensor (351), a fourth tail gas outlet pipe (352) and a fourth vent valve (353); 6) comprising a fifth pressure sensor (361), a fifth tail gas outlet pipe (362) and a fifth vent valve (363), wherein the fifth pressure sensor (361) and the fifth tail gas outlet pipe (362) are both arranged on the waste liquid tank (26), and the fifth vent valve (363) is arranged on the fifth tail gas outlet pipe (362); the second temperature control unit (37) comprises a second temperature sensor (371) and a water supply valve (372), the second temperature sensor (371) and the water inlet pipe (29) are arranged on the hydrolysis tank (28), and the water supply valve (372) is arranged on the water inlet pipe (29).

11. The comprehensive utilization system for slag discharged from cold hydrogenation according to claim 10, characterized in that: The first liquid outlet pipe (14) and the second liquid outlet pipe (18) are respectively provided with a first tower bottom pump (33) and a second tower bottom pump (34).