Aluminum gel adsorbent activation system and method
By controlling the activated aluminum tetrachloride gel adsorbent with nitrogen bubbling, the problem of temperature rise during the activation process was solved, achieving temperature control and resource recovery, extending the service life of the adsorbent and shortening the activation cycle.
Patent Information
- Application Number
- CN202511473354.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-15
- Publication Date
- 2025-12-05
AI Technical Summary
In the activation process of aluminum gel adsorbents in the prior art, silicon tetrachloride reacts violently with moisture, which destroys the adsorbent skeleton structure, causes the temperature to rise and cool down slowly, and affects the adsorption effect and service life.
The activation rate of silicon tetrachloride is controlled by nitrogen bubbling, and the reaction temperature is controlled by adjusting the nitrogen flow rate. Gas-phase silicon tetrachloride is used for activation, and residual silicon tetrachloride and trichlorosilane are recovered by condensation, thus realizing the secondary utilization of resources.
Effective control of activation temperature protects the adsorbent skeleton, shortens the activation cycle, improves resource utilization, and extends the service life of the adsorbent.
Smart Images
Figure CN121060232A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of trichlorosilane boron removal, and particularly relates to an aluminum gel adsorbent activation system and method. BACKGROUND
[0002] Polysilicon is an important material for large-scale semiconductor industry and photovoltaic industry, and the purity of the raw material is crucial to the final production. The current preparation process removes boron from the trichlorosilane raw material to improve the purity of trichlorosilane.
[0003] In the related art, the boron removal device uses relatively stable aluminum gel adsorbent for boron removal. Before the adsorbent is put into use, it needs to be activated by using silicon tetrachloride with relatively weak activity. Silicon tetrachloride reacts with water in the adsorbent to reduce the activity of the adsorbent, so that the adsorbent can be in a stable state when put into use.
[0004] In the related art, liquid silicon tetrachloride is used for aluminum gel adsorbent activation, and the feeding speed is difficult to control, resulting in a relatively violent reaction between silicon tetrachloride and water. The adsorption column produces a sharp temperature rise. On the one hand, the high temperature can damage the skeleton structure of the adsorbent, resulting in poor adsorption effect and greatly reducing the service life of the adsorbent. On the other hand, the adsorption column cools down slowly after overheating, resulting in a long adsorbent activation period. SUMMARY
[0005] In order to overcome the deficiencies in the prior art, the application provides an aluminum gel adsorbent activation system and method.
[0006] To solve the above technical problems, the technical scheme adopted by the application is as follows: In a first aspect, an aluminum gel adsorbent activation system is provided, comprising a nitrogen gas input path for discharging air, a nitrogen gas bubbling path for activating aluminum gel adsorbent, a silicon tetrachloride liquid input path, a silicon tetrachloride gas input path for discharging nitrogen gas, and an adsorption column. The adsorption column is provided with a top outlet and a bottom inlet. The nitrogen gas bubbling path comprises a bubbling tank for storing silicon tetrachloride liquid. The bubbling tank is provided with a first inlet for introducing silicon tetrachloride liquid, a second inlet for introducing nitrogen gas, and a bubbling tank outlet for nitrogen gas bubbling to carry out silicon tetrachloride gas. The outlet of the nitrogen gas input path is connected with the bottom inlet of the adsorption column, the outlet of the nitrogen gas bubbling path is connected with the bottom inlet of the adsorption column, the outlet of the silicon tetrachloride liquid input path is connected with the first inlet of the bubbling tank, and the outlet of the silicon tetrachloride gas input path is in communication with the nitrogen gas input path.
[0007] In the embodiment, the activation of the adsorbent by the gaseous silicon tetrachloride is achieved by nitrogen bubbling, the bubbling speed can be controlled by adjusting the nitrogen flow rate, thereby controlling the silicon tetrachloride gas flow rate out of the bubbling tank, and further controlling the activation speed of the adsorbent. The reaction between the silicon tetrachloride and the moisture in the adsorbent is controllable, thereby ensuring that the adsorption column is heated gently, the overall temperature is low, and the skeleton structure of the adsorbent is not damaged by high temperature; the cooling speed is fast, and the activation period is shortened.
[0008] In some embodiments, the nitrogen input passage includes pipeline one, pipeline two, pipeline seven and pipeline nine for providing nitrogen, the outlet of pipeline one is connected to one end of pipeline two, the other end of pipeline two is connected to one end of pipeline seven, the other end of pipeline seven is communicated with pipeline nine, and one end of pipeline nine is connected to the bottom inlet of the adsorption column.
[0009] The nitrogen bubbling passage further includes pipeline three and pipeline eight, one end of pipeline three is communicated with pipeline two, and the other end is connected to the second inlet of the bubbling tank, one end of pipeline eight is connected to the outlet of the bubbling tank, and the other end of pipeline eight is connected to pipeline nine.
[0010] The silicon tetrachloride gas input passage includes pipeline five and pipeline six for providing silicon tetrachloride, pipeline five is connected to one end of pipeline six, and the other end of pipeline six is communicated with pipeline seven.
[0011] The silicon tetrachloride liquid input passage includes pipeline four, one end of pipeline four is communicated with pipeline six, and the other end of pipeline four is connected to the first inlet of the bubbling tank.
[0012] In some embodiments, the aluminum gel adsorbent activation system further includes pipeline ten for providing trichlorosilane, pipeline ten is communicated with pipeline six, for transporting trichlorosilane into the adsorption column to discharge the silicon tetrachloride gas in the adsorption column and remove boron impurities carried by the trichlorosilane.
[0013] In some embodiments, the aluminum gel adsorbent activation system further includes pipeline twelve, a storage tank and a pressure pump, the top outlet of the adsorption column is connected to the inlet of the storage tank through pipeline twelve, for collecting the silicon tetrachloride gas discharged from the adsorption column and the trichlorosilane before the boron impurities are removed; and the pressure pump is connected to the outlet of the storage tank, for providing transportation power.
[0014] In the embodiment, the residual silicon tetrachloride in the adsorption column after the activation is discharged by the trichlorosilane introduced, and is recovered and reused together with the trichlorosilane.
[0015] In some embodiments, the aluminum gel adsorbent activation system further includes pipeline thirteen connected to the top outlet of the adsorption column, for collecting the trichlorosilane after the boron impurities are removed for subsequent use.
[0016] In some embodiments, the aluminum gel adsorbent activation system further comprises line eleven, which is connected to the top outlet of the adsorption column for separating and recovering silicon tetrachloride.
[0017] In this embodiment, the residual silicon tetrachloride in the activation reaction process is condensed and recovered, improving resource utilization.
[0018] In a second aspect, an aluminum gel adsorbent activation method is provided, based on the aluminum gel adsorbent activation system, the method comprising: Nitrogen is introduced from line one, and is introduced into the adsorption column through line two, line seven, and line nine to discharge air until the dew point is lower than -40℃ and the micro-oxygen is less than 20 ppm, and the discharge is completed; Silicon tetrachloride liquid is introduced from line five, and is introduced into the bubbling tank through line six and line four; Nitrogen is introduced into the bubbling tank with silicon tetrachloride liquid through line one, line two, and line three, and silicon tetrachloride gas is brought out of the bubbling tank by bubbling, and is introduced into the adsorption column through line eight and line nine, and the silicon tetrachloride gas activates the aluminum gel adsorbent, and is discharged from the top outlet of the adsorption column, and is condensed and recovered in line eleven; After the activation is completed, silicon tetrachloride liquid is introduced from line five, and is introduced into the adsorption column through line six, line seven, and line nine to discharge nitrogen, and is discharged from the top outlet of the adsorption column, and is introduced into the storage tank through line twelve for subsequent recycling.
[0019] In some embodiments, the method for judging the completion of activation comprises: The temperature of the adsorption column is measured, and the continuous decrease of the temperature of the adsorption column indicates that the silicon tetrachloride no longer activates the aluminum gel adsorbent to release heat, and the activation is completed; In another embodiment, the contents of silicon tetrachloride gas in line eight and line eleven are compared, and the contents of silicon tetrachloride gas in line eight and line eleven are the same, indicating that the silicon tetrachloride no longer activates the aluminum gel adsorbent to consume silicon tetrachloride, and the activation is completed.
[0020] In some embodiments, after the nitrogen is discharged, trichlorosilane liquid is introduced from line ten, and is introduced into the adsorption column through line six, line seven, and line nine to discharge silicon tetrachloride, and is discharged from the top outlet of the adsorption column, and is introduced into the storage tank through line twelve; the mixture of trichlorosilane and silicon tetrachloride in the storage tank flows out from the outlet of the storage tank, and is continuously transported by a pressure pump for subsequent recycling.
[0021] After the silicon tetrachloride is discharged, the trichlorosilane begins to be adsorbed to remove boron impurities, and the trichlorosilane after the removal of boron impurities is collected through line thirteen for use in subsequent sections.
[0022] Preferably, the method keeps the activation temperature at 80-100 DEG C. It is beneficial to ensure the activation efficiency, prolong the service life of the adsorbent and shorten the activation period.
[0023] Beneficial effects: the aluminum gel adsorbent activation system provided by the application has the following advantages: 1. The nitrogen bubbling method is used to realize the activation of the adsorbent by gaseous silicon tetrachloride, which is beneficial to control the activation reaction speed, and further control the activation temperature, protect the adsorbent skeleton from high temperature damage, prolong the service life of the adsorbent, make the activation reaction more stable, the overall temperature of the adsorption column is lower, and the activation period is shortened. 2. The silicon tetrachloride and trichlorosilane used in the activation process are separated and recovered after being discharged, the secondary use of resources saves the production cost. BRIEF DESCRIPTION OF DRAWINGS
[0024] Figure 1 It is the principle diagram of the adsorbent activation system of the embodiment of the application. Figure 2 It is the principle diagram of the trichlorosilane boron removal system of the embodiment of the application.
[0025] The reference signs are described as follows: the bubbling tank 1, the first inlet 10, the second inlet 102, the bubbling tank outlet 103, the adsorption column 2, the top outlet 201, the bottom inlet 202, the pipeline one 3, the pipeline two 4, the pipeline three 5, the pipeline four 6, the pipeline five 7, the pipeline six 8, the pipeline seven 9, the pipeline eight 10, the pipeline nine 11, the pipeline ten 12, the pipeline eleven 13, the pipeline twelve 14, the pipeline thirteen 15, the storage tank 16, and the pressure pump 17. DETAILED DESCRIPTION
[0026] The technical solutions in the embodiments of the application are clearly and completely described below in combination with the drawings in the embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments of the application. Based on the embodiments of the application, all other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the application.
[0027] The foregoing is considered as illustrative only of the principles of the application. Further, since numerous modifications and changes will readily occur to those skilled in the art, it is not desired to limit the application to the exact construction and practice described. Accordingly, all such variations are intended to be included within the scope of the present application as defined in the following claims, along with full equivalents thereof.
[0028] In the description of the present application, the meaning of a plurality of one or more, the meaning of a plurality of two or more, greater than, less than, more than, etc. are understood to not include the number itself, and the meaning of above, below, within, etc. are understood to include the number itself. If it is described as first, second, etc., it is only for the purpose of distinguishing the technical features being described and cannot be understood as indicating or implying relative importance or implying the number of technical features indicated or the order of the technical features indicated.
[0029] In the description of the present application, the description of the terms "one embodiment", "some embodiments", "exemplary embodiment", "example", "specific example", or "some examples" means that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present application. In the present specification, the exemplary description of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.
[0030] The present application will be further described below with reference to specific embodiments.
[0031] Embodiment 1: As shown in Figure 1 and Figure 2 An aluminum gel adsorbent activation system, including a nitrogen gas input passage for discharging air, a nitrogen gas bubbling passage for activating aluminum gel adsorbent, a silicon tetrachloride liquid input passage, a silicon tetrachloride gas input passage for discharging nitrogen gas, and an adsorption column 2 provided with a top outlet 201 and a bottom inlet 202, the nitrogen gas bubbling passage including a bubbling tank 1 for storing silicon tetrachloride liquid, the bubbling tank 1 being provided with a first inlet 101 for introducing silicon tetrachloride liquid, a second inlet 102 for introducing nitrogen gas, and a bubbling tank outlet 103 for nitrogen gas bubbling to carry out silicon tetrachloride gas; The nitrogen input passage outlet is connected with the bottom inlet 202 of the adsorption column 2, the nitrogen bubbling passage outlet is connected with the bottom inlet 202 of the adsorption column 2, the silicon tetrachloride liquid input passage outlet is connected with the first inlet 101 of the bubbling tank 1, and the silicon tetrachloride gas input passage outlet is communicated with the nitrogen input passage.
[0032] In some embodiments, the nitrogen input passage comprises pipelines one 3, two 4, seven 9 and nine 11 for providing nitrogen, the outlet of the pipeline one 3 is connected with one end of the pipeline two 4, the other end of the pipeline two 4 is connected with one end of the pipeline seven 9, the other end of the pipeline seven 9 is communicated with the pipeline nine 11, and the pipeline nine 11 is connected with the bottom inlet 202 of the adsorption column 2.
[0033] The nitrogen bubbling passage further comprises pipelines three 5 and eight 10, one end of the pipeline three 5 is communicated with the pipeline two 4, and the other end is connected with the second inlet 102 of the bubbling tank 1, one end of the pipeline eight 10 is connected with the bubbling tank outlet 103, and the other end of the pipeline eight 10 is connected with the pipeline nine 11.
[0034] The silicon tetrachloride gas input passage comprises pipelines five 7 and six 8 for providing silicon tetrachloride, the pipeline five 7 is connected with one end of the pipeline six 8, and the other end of the pipeline six 8 is communicated with the pipeline seven 9. In the embodiment, the silicon tetrachloride gas input passage shares the pipeline seven 9 and the pipeline nine 11 with the nitrogen input passage, and the silicon tetrachloride gas is transported into the adsorption column 2 to discharge the nitrogen.
[0035] The silicon tetrachloride liquid input passage comprises the pipeline four 6, one end of the pipeline four 6 is communicated with the pipeline six 8, and the other end of the pipeline four 6 is connected with the first inlet 101 of the bubbling tank 1.
[0036] In the embodiment, the silicon tetrachloride liquid input passage shares the pipeline five 7 and the pipeline six 8 with the silicon tetrachloride gas input passage, and the silicon tetrachloride liquid enters from the pipeline five 7 and enters the bubbling tank 1 from the pipeline four 6.
[0037] In some embodiments, the aluminum gel adsorbent activation system further comprises a pipeline ten 12 for providing trichlorosilane, the pipeline ten 12 is communicated with the pipeline six 8, and is used for transporting the trichlorosilane into the adsorption column 2 to discharge the silicon tetrachloride gas in the adsorption column 2 and remove the boron impurities carried by the trichlorosilane.
[0038] In some embodiments, the aluminum gel adsorbent activation system further comprises a pipeline twelve 14, a storage tank 16 and a pressure pump 17, the top outlet 201 of the adsorption column 2 is connected with the inlet of the storage tank 16 through the pipeline twelve 14, and is used for collecting the silicon tetrachloride gas discharged from the adsorption column 2 and the trichlorosilane before the boron impurities are removed; and the pressure pump 17 is connected with the outlet of the storage tank 16, and is used for providing transportation power.
[0039] In the present embodiment, the residual silicon tetrachloride in the adsorption column 2 after the activation is discharged by the trichlorosilane introduced and is separated and recovered together with the trichlorosilane and is then reused.
[0040] In some embodiments, the aluminum gel adsorbent activation system further comprises a pipeline thirteen 15 connected with the top outlet 201 of the adsorption column 2 for collecting the trichlorosilane after the boron impurities are removed for subsequent use.
[0041] In some embodiments, the aluminum gel adsorbent activation system further comprises a pipeline eleven 13 connected with the top outlet 201 of the adsorption column 2 for separating and recovering the silicon tetrachloride. In the present embodiment, the residual silicon tetrachloride in the activation reaction process is condensed and recovered, improving the resource utilization rate.
[0042] Embodiment 2: An aluminum gel adsorbent activation method based on the aluminum gel adsorbent activation system described in Embodiment 1, the method comprising: Nitrogen is introduced from the pipeline one 3, enters the adsorption column 2 through the pipeline two 4, the pipeline seven 9 and the pipeline nine 11 to discharge air until the dew point is lower than -40℃ and the micro-oxygen is less than 20 ppm, and the discharge is completed; Silicon tetrachloride liquid is introduced from the pipeline five 7, enters the bubbling tank 1 through the pipeline six 8 and the pipeline four 6; Nitrogen enters the bubbling tank 1 with silicon tetrachloride liquid through the pipeline one 3, the pipeline two 4 and the pipeline three 5, silicon tetrachloride gas is brought out of the bubbling tank 1 by bubbling, enters the adsorption column 2 through the pipeline eight 10 and the pipeline nine 11, the aluminum gel adsorbent is activated by the silicon tetrachloride gas, and then is discharged from the top outlet 201 of the adsorption column 2, enters the pipeline eleven 13 and is condensed and recovered; After the activation is completed, silicon tetrachloride liquid is introduced from the pipeline five 7, enters the adsorption column 2 through the pipeline six 8, the pipeline seven 9 and the pipeline nine 11 to discharge nitrogen, and then is discharged from the top outlet 201 of the adsorption column 2, enters the storage tank 16 through the pipeline twelve 14 for subsequent recovery and utilization.
[0043] The judgment method for the completion of the activation comprises: The temperature of the adsorption column 2 is measured, and the temperature of the adsorption column 2 continues to drop, indicating that the silicon tetrachloride no longer activates and releases heat to the aluminum gel adsorbent, and the activation is completed. In another embodiment, the contents of the silicon tetrachloride gas in the pipeline eight 10 and the pipeline eleven 13 are compared, and the contents of the silicon tetrachloride gas in the pipeline eight 10 and the pipeline eleven 13 are the same, indicating that the silicon tetrachloride no longer activates and consumes the silicon tetrachloride to the aluminum gel adsorbent, and the activation is completed.
[0044] In some embodiments, after the nitrogen gas is discharged, trichlorosilane liquid is introduced from line 12 into the adsorption column 2 through line 6, line 7 and line 9, and the silicon tetrachloride is discharged from the adsorption column 2, and then discharged from the top outlet 201 of the adsorption column 2 through line 14 into the storage tank 16; the trichlorosilane and silicon tetrachloride mixture in the storage tank 16 is discharged from the outlet of the storage tank 16, and is continuously transported by the power of the pressure pump 17 for subsequent recycling.
[0045] After the silicon tetrachloride is discharged, the trichlorosilane is adsorbed to remove boron impurities, and the trichlorosilane after the removal of boron impurities is collected through line 15 for subsequent use.
[0046] Preferably, the method maintains the activation temperature at 80-100°C. This is advantageous to ensure the activation efficiency, prolong the service life of the adsorbent, and shorten the activation period.
[0047] The above is only the preferred embodiment of the present application, and it should be noted that for those skilled in the art, without departing from the principles of the present application, a number of improvements and refinements can be made, and these improvements and refinements should also be considered within the scope of protection of the present application.
Claims
1. An aluminum gel sorbent activation system characterized by, The system comprises a nitrogen input passage for discharging air, a nitrogen bubbling passage for activating aluminum gel adsorbent, a silicon tetrachloride liquid input passage, a silicon tetrachloride gas input passage for discharging nitrogen, and an adsorption column (2), wherein the adsorption column (2) is provided with a top outlet (201) and a bottom inlet (202), the nitrogen bubbling passage comprises a bubbling tank (1) for storing silicon tetrachloride liquid, the bubbling tank (1) is provided with a first inlet (101) for introducing silicon tetrachloride liquid, a second inlet (102) for introducing nitrogen, and a bubbling tank outlet (103) for nitrogen bubbling to carry out silicon tetrachloride gas; The outlet of the nitrogen input passage is connected with the bottom inlet (202) of the adsorption column (2), the outlet of the nitrogen bubbling passage is connected with the bottom inlet (202) of the adsorption column (2), the outlet of the silicon tetrachloride liquid input passage is connected with the first inlet (101) of the bubbling tank (1), and the outlet of the silicon tetrachloride gas input passage is communicated with the nitrogen input passage.
2. The aluminum gel adsorbent activation system of claim 1, wherein, The nitrogen input passage comprises a pipeline one (3) for providing nitrogen, a pipeline two (4), a pipeline seven (9), and a pipeline nine (11), the outlet of the pipeline one (3) is connected with one end of the pipeline two (4), the other end of the pipeline two (4) is connected with one end of the pipeline seven (9), the other end of the pipeline seven (9) is communicated with the pipeline nine (11), and the pipeline nine (11) is connected with the bottom inlet (202) of the adsorption column (2); The nitrogen bubbling passage further comprises a pipeline three (5) and a pipeline eight (10), one end of the pipeline three (5) is communicated with the pipeline two (4), and the other end is connected with the second inlet (102) of the bubbling tank (1), one end of the pipeline eight (10) is connected with the bubbling tank outlet (103), and the other end of the pipeline eight (10) is connected with the pipeline nine (11); The silicon tetrachloride gas input passage comprises a pipeline five (7) for providing silicon tetrachloride and a pipeline six (8), the pipeline five (7) is connected with one end of the pipeline six (8), and the other end of the pipeline six (8) is communicated with the pipeline seven (9); The silicon tetrachloride liquid input passage comprises a pipeline four (6), one end of the pipeline four (6) is communicated with the pipeline six (8), and the other end of the pipeline four (6) is connected with the first inlet (101) of the bubbling tank (1).
3. The aluminum gel sorbent activation system of claim 2, wherein, The aluminum gel adsorbent activation system further comprises a pipeline ten (12) for providing trichlorosilane, the pipeline ten (12) is communicated with the pipeline six (8), for transporting trichlorosilane into the adsorption column (2) to discharge silicon tetrachloride gas in the adsorption column (2) and remove boron impurities carried by the trichlorosilane.
4. The aluminum gel sorbent activation system of claim 3, wherein, The aluminum gel adsorbent activation system further comprises a pipeline twelve (14), a storage tank (16), and a pressure pump (17), the top outlet (201) of the adsorption column (2) is connected with an inlet of the storage tank (16) through the pipeline twelve (14), for collecting silicon tetrachloride gas discharged from the adsorption column (2) and trichlorosilane before removing boron impurities, and the pressure pump (17) is connected with an outlet of the storage tank (16), for providing transportation power.
5. The aluminum gel sorbent activation system of claim 3, wherein, The aluminum gel adsorbent activation system further comprises pipeline thirteen (15) connected with the top outlet (201) of the adsorption column (2) for collecting trichlorosilane after removal of boron impurities for subsequent use.
6. The aluminum gel sorbent activation system of claim 1, wherein, The aluminum gel adsorbent activation system further comprises pipeline eleven (13) connected with the top outlet (201) of the adsorption column (2) for separating and recovering silicon tetrachloride.
7. A method of activating an aluminum gel adsorbent based on the system for activating an aluminum gel adsorbent according to any one of claims 1 to 6, characterized by, The method comprises the following steps: Nitrogen is introduced from pipeline one (3) and discharged into the adsorption column (2) through pipeline two (4), pipeline seven (9) and pipeline nine (11) to discharge air until the dew point is lower than-40℃ and the oxygen content is less than 20 ppm, and the discharging is completed; Silicon tetrachloride liquid is introduced from pipeline five (7) and enters the bubbling tank (1) through pipeline six (8) and pipeline four (6); Nitrogen is introduced into the bubbling tank (1) containing silicon tetrachloride liquid through pipeline one (3), pipeline two (4) and pipeline three (5), silicon tetrachloride gas is brought out of the bubbling tank (1) by bubbling, enters the adsorption column (2) through pipeline eight (10) and pipeline nine (11), the aluminum gel adsorbent is activated by the silicon tetrachloride gas, and then is discharged from the top outlet (201) of the adsorption column (2) and enters pipeline eleven (13) to be condensed and recovered; After the activation is completed, silicon tetrachloride liquid is introduced from pipeline five (7) and enters the adsorption column (2) through pipeline six (8), pipeline seven (9) and pipeline nine (11) to discharge nitrogen, and then is discharged from the top outlet (201) of the adsorption column (2) and enters the storage tank (16) through pipeline twelve (14) for subsequent recovery and utilization.
8. The aluminum gel adsorbent activation method of claim 7, wherein, The judgment method for completion of the activation comprises: The temperature of the adsorption column (2) is measured, and the temperature of the adsorption column (2) continues to drop, indicating that the silicon tetrachloride is no longer activated by the aluminum gel adsorbent to release heat, and the activation is completed; And / or, the contents of silicon tetrachloride gas in pipeline eight (10) and pipeline eleven (13) are compared, and the contents of silicon tetrachloride gas in pipeline eight (10) and pipeline eleven (13) are the same, indicating that the silicon tetrachloride is no longer activated by the aluminum gel adsorbent to consume silicon tetrachloride, and the activation is completed.
9. The aluminum gel adsorbent activation method of claim 7, wherein, After the nitrogen is discharged, trichlorosilane liquid is introduced from pipeline ten (12) and enters the adsorption column (2) through pipeline six (8), pipeline seven (9) and pipeline nine (11) to discharge silicon tetrachloride, and then is discharged from the top outlet (201) of the adsorption column (2) and enters the storage tank (16) through pipeline twelve (14); the mixture of trichlorosilane and silicon tetrachloride in the storage tank (16) flows out from the outlet of the storage tank (16) and is continuously transported by a pressure pump (17) for subsequent recovery and utilization; After the silicon tetrachloride is discharged, the trichlorosilane is subjected to adsorption to remove boron impurities, and the trichlorosilane after removal of boron impurities is collected through pipeline thirteen (15) for use in subsequent sections.
10. The aluminum gel adsorbent activation method of claim 7 or 8, wherein, The method keeps the activation temperature at 80-100℃.