Amino silane purification process and device capable of efficiently removing chloride ions

Abstract

The invention relates to the technical field of semiconductor chips, and particularly discloses an aminosilane purification process capable of efficiently removing chloride ions, which comprises a metal activation tower and comprises the following steps: S1, activation column filling: uniformly filling an activation column in the metal activation tower with unactivated magnesium chips; s2, HCl gas activation and demolding: heating the activation column to 200 DEG C, introducing HCl gas into the activation column, maintaining an activation reaction for 1 h, and discharging water generated by reaction of the HCl gas and magnesium oxide on the surface of magnesium along with tail gas in a gaseous form. According to the amino silane purification process capable of efficiently removing the chloride ions, magnesium is activated, so that high-activity sites are formed on the surface of the magnesium, then a replacement reaction between the chloride ions and the magnesium is promoted, and magnesium chloride precipitates are generated and separated from a system; by arranging the activation tower equipment, waste gas can be blown away while magnesium oxide is effectively removed, meanwhile, in the subsequent activation stage, magnesium chloride powder can be blown, and magnesium chloride mixed in magnesium chips can be effectively stripped.

Description

Technical Field

[0001] This invention relates to the field of semiconductor chip technology, and more specifically to an aminosilane purification process that can efficiently remove chloride ions. Background Technology

[0002] Aminosilanes, such as diisopropylaminosilane, bis(diethylamino)silane, and bis(tert-butylamino)silane, are key precursors for atomic layer deposition (ALD) and chemical vapor deposition (CVD) processes in advanced semiconductor chip manufacturing. These applications have extremely stringent purity requirements for the precursors; the chloride ion content must be strictly controlled at the ppm or even ppb level, as chloride ions can lead to device performance degradation and decreased reliability. In conventional synthesis processes, the byproduct hydrogen chloride can react with amines to form amine hydrochloride or introduce chloride ions in other forms, resulting in a decrease in product purity.

[0003] Currently, conventional methods for removing chloride ions from aminosilanes mainly include vacuum distillation and physical adsorption. While vacuum distillation is effective, it is inefficient for systems with boiling points close to the decomposition temperature of amine hydrochlorides, and it is also energy-intensive and time-consuming. Physical adsorption suffers from limited adsorption capacity and difficulties in adsorbent regeneration.

[0004] In addition, some studies have attempted to use chemical neutralization methods, such as sodium amide, sodium hydride, sodium ethoxide, and sodium methoxide. While these reagents are effective at removing chlorine, they are themselves highly nucleophilic and reactive. During the chlorination process, they may react with the target aminosilane, introducing new impurities or altering the chemical structure of the main molecule, leading to the destruction of the target product and a significant reduction in yield.

[0005] Therefore, there is an urgent need in this field to develop a purification method that can achieve deep dechlorination, absolutely guarantee the integrity of the aminosilane molecular structure, and is suitable for industrial production. Summary of the Invention

[0006] The purpose of this invention is to provide an aminosilane purification process that can efficiently remove chloride ions, thereby overcoming the aforementioned shortcomings of the prior art.

[0007] To achieve the above objectives, the present invention provides the following technical solution:

[0008] An efficient process for purifying aminosilanes by removing chloride ions includes a metal activation tower, and the steps are as follows:

[0009] S1: Activation column loading: Unactivated magnesium shavings are uniformly loaded into the activation column in the metal activation tower and replaced with inert gas to make the system in an inert gas state.

[0010] S2: HCl gas activation and descaling: The activation column is heated to 200℃, and HCl gas with a purity of ≥99.9% is introduced into the activation column. The activation reaction is maintained for 1 hour. The water generated by the reaction of HCl gas with magnesium oxide on the magnesium surface is discharged in gaseous form with the tail gas.

[0011] S3: During the activation stage, the vibrator is turned on and the activation column is controlled to rotate at a set angle every set time to make the HCl gas react evenly with the unactivated magnesium shavings.

[0012] S4: Magnesium purification after activation: Stop the HCl gas flow, purge the activation column with inert gas for 3 hours, maintain the purging temperature at 200℃, and remove residual HCl gas, trace amounts of gaseous water and trace amounts of magnesium chloride.

[0013] S5: Purification stage. Control the rotating cylinder to the tilted position, turn on the vibrator, and the powdered magnesium chloride will fall out and be blown out of the activation column by inert gas.

[0014] S6: Subsequently, the mixture was cooled to room temperature under argon protection. During the cooling process, the argon flow rate was reduced to 0.2 ~ 0.4 L / min, and finally activated magnesium was obtained.

[0015] S7: Under anhydrous and oxygen-free conditions, the aminosilane raw material containing chloride ions is mixed with the above-mentioned activated magnesium, and then heated and stirred for 10-12 hours. After the reaction is completed, it is distilled under reduced pressure to obtain low-chlorine aminosilane.

[0016] Furthermore, the flow rate of the HCl gas is controlled at 0.5 L / min, and the flow rate of the inert gas is controlled at 3 L / min.

[0017] Furthermore, the hydrogen chloride gas in S2 is diluted with an inert gas before being introduced, with a dilution concentration of 5~20 vol%.

[0018] Furthermore, the molar ratio of the activated magnesium to the chlorine atoms in the aminosilane raw material is 2-4:1.

[0019] Furthermore, the heating temperature in S7 is 40~50℃.

[0020] Furthermore, the temperature of the vacuum distillation is 50~60℃, and the vacuum degree is below 1kPa.

[0021] An aminosilane purification device capable of efficiently removing chloride ions is provided, applied to the aforementioned aminosilane purification process capable of efficiently removing chloride ions. The metal activation tower includes a tower body and an activation column disposed inside the tower body. The activation column is provided with a packing component, which includes a rotating cylinder. A perforated frame is fixedly connected inside the rotating cylinder. Multiple gas channels are formed between the inner cavity of the rotating cylinder and the perforated frame. After the gas fully contacts the packing through the perforated frame, it carries the impurities and is discharged from the activation column.

[0022] Furthermore, the activation column is also equipped with a rotating component, and an annular groove is opened on the rotating drum. A sealing ring is rotatably connected in the annular groove, and an air inlet pipe and an air outlet pipe are fixedly connected to the sealing ring. A reduction motor is fixedly connected to the bottom of the activation column, and the output end of the reduction motor is fixedly connected to the rotating drum located at the bottom. Telescopic components are provided between adjacent rotating drums. The reduction motor drives multiple rotating drums to rotate at a set angle through multiple transmission components.

[0023] Furthermore, multiple fixing rings are fixedly connected inside the activation column, and multiple vibrators are fixedly connected between the fixing rings and the rotating cylinder.

[0024] Furthermore, a hydraulic rod is installed inside the activation column, with its end in contact with the inside of the activation column. A support rod is fixedly connected to the outside of the activation column, and the support rod is rotatably connected to the inner wall of the tower body. When the hydraulic rod is activated, it drives the activation column to tilt.

[0025] In the above technical solution, the aminosilane purification process for efficiently removing chloride ions provided by the present invention has the following beneficial effects:

[0026] By activating magnesium, highly active sites are formed on its surface, which promotes the displacement reaction between chloride ions and magnesium, generating magnesium chloride precipitate, which is then separated from the system. This process avoids the attack of strong nucleophiles on the aminosilane structure, effectively maintaining the chemical stability of the main molecule. Furthermore, the reaction conditions are mild, the operation is simple, and it is suitable for large-scale industrial production, significantly improving product purity and yield.

[0027] By setting up an air-blowing activation method and using an activation tower, magnesium oxide can be effectively removed while waste gas is blown away. In the subsequent activation stage, magnesium chloride powder can also be purged, effectively stripping magnesium chloride mixed in with magnesium shavings. This ensures that unactivated magnesium is fully in contact with HCl gas, and that the contact time between each part of magnesium and HCl gas is constant, ensuring that magnesium is not consumed. It also efficiently removes solid impurities while removing waste gas impurities, and the reaction does not introduce new impurities.

[0028] It should be understood that the foregoing general description and the following detailed description are exemplary and illustrative only, and are not intended to limit this disclosure.

[0029] This application provides an overview of various implementations or examples of the technology described in this disclosure, and is not a full disclosure of the entire scope or all features of the disclosed technology. Attached Figure Description

[0030] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in this invention. For those skilled in the art, other drawings can be obtained based on these drawings.

[0031] Figure 1 This is a schematic diagram of the external structure of the tower body provided in an embodiment of the present invention;

[0032] Figure 2 This is a schematic diagram of the external structure of the activation column provided in an embodiment of the present invention;

[0033] Figure 3 This is a schematic diagram of the activation column from another perspective provided in an embodiment of the present invention;

[0034] Figure 4 A schematic diagram of the external structure of the rotating drum provided in an embodiment of the present invention;

[0035] Figure 5 This is a schematic diagram of the internal cracking structure of the rotating drum provided in an embodiment of the present invention;

[0036] Figure 6 This is a schematic diagram of the hollow frame structure provided in an embodiment of the present invention;

[0037] Figure 7 This is a schematic diagram of a preferred embodiment of the hollow frame provided in this invention.

[0038] Explanation of reference numerals in the attached figures:

[0039] 1. Tower body; 2. Activation column; 3. Packing components; 31. Rotary drum; 32. Hollow frame; 33. Gas channel; 34. Smooth plate; 35. Baffle plate; 4. Rotating components; 41. Sealing ring; 42. Inlet pipe; 43. Outlet pipe; 44. Gear motor; 45. Telescopic component; 5. Fixing ring; 6. Vibrator; 7. Hydraulic rod; 8. Support rod; 9. Sealing plate; 10. Electromagnet; 11. Connecting rod; 12. Feed pipe; 13. Discharge pipe; 14. Unloading pipe. Detailed Implementation

[0040] To make the objectives, technical solutions, and advantages of the embodiments of this disclosure clearer, the technical solutions of the embodiments of this disclosure will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this disclosure. All other embodiments obtained by those skilled in the art based on the described embodiments of this disclosure without creative effort are within the scope of protection of this disclosure.

[0041] Please refer to 1-9, an aminosilane purification process for efficient removal of chloride ions, including a metal activation tower, the steps of which are as follows:

[0042] Activation column loading: Unactivated magnesium shavings are uniformly loaded into the activation column of the metal activation tower and replaced with inert gas to make the system in an inert gas state.

[0043] HCl gas activation and descaling: The activation column is heated to 200℃, and HCl gas with a purity of ≥99.9% is introduced into the activation column. The gas flow rate is controlled at 0.5L / min, and the activation reaction is maintained for 1h. The water generated by the reaction of HCl gas with magnesium oxide on the magnesium surface is discharged in gaseous form with the tail gas.

[0044] During the activation phase, the vibrator is turned on, and the activation column is controlled to rotate at a set angle every set time to ensure that the HCl gas reacts evenly with the unactivated magnesium shavings.

[0045] Magnesium purification after activation: Stop the HCl gas flow, control the inert gas flow rate at 3 L / min, purge the activation column with inert gas for 3 hours, maintain the purging temperature at 200℃, and remove residual HCl gas, trace amounts of gaseous water and trace amounts of magnesium chloride.

[0046] During the purification stage, the movable cylinder is rotated to an inclined position, the vibrator is turned on, and the powdered magnesium chloride is shaken out and then purged out of the activation column by inert gas.

[0047] The magnesium was then cooled to room temperature under argon protection. During the cooling process, the argon flow rate was reduced to 0.2-0.4 L / min, and finally activated magnesium was obtained.

[0048] Under anhydrous and oxygen-free conditions, an aminosilane raw material containing chloride ions is mixed with the above-mentioned activated magnesium, and then heated and stirred for 10-12 hours at a heating temperature of 40-50°C. After the reaction is completed, the mixture is distilled under reduced pressure to obtain a low-chlorine aminosilane.

[0049] Specifically, hydrogen chloride gas is diluted with an inert gas before being introduced, with a dilution concentration of 5-20 vol.

[0050] The molar ratio of the activated magnesium to the chlorine atoms in the aminosilane raw material is 2-4:1.

[0051] The vacuum distillation temperature is 50~60℃, and the vacuum degree is below 1kPa.

[0052] Example 1:

[0053] Control group – using unactivated ordinary magnesium filings

[0054] 1. Dechlorination of bis(diethylamino)silane: Add 2 kg of crude bis(diethylamino)silane with a chlorine content of 56 ppm to the reaction flask, then add 0.5 g of magnesium shavings, and then heat to 40°C and stir for 10 hours.

[0055] 2. After the reaction is complete, the mixture is heated to 50-60℃ and subjected to vacuum distillation at a pressure below 1 kPa to obtain 1.9 kg of bis(diethylamino)silane.

[0056] 3. The bis(diethylamino)silane obtained after dechlorination was found to have a chlorine content of 13 ppm. GC-MS analysis showed that there were obvious siloxane hydrolysis byproducts.

[0057] Next, we will use activated magnesium for our experiment.

[0058] 1. Activation column loading: Under anhydrous and oxygen-free conditions, 2 kg of magnesium shavings are filled into a corrosion-resistant Hastelloy activation column, and then connected to the gas system, which is purged with high-purity nitrogen.

[0059] 2. HCl gas activation and membrane removal: The activation column is heated to 200℃, and then 10 vol% anhydrous HCl gas diluted with high-purity nitrogen is introduced at a total flow rate of 0.5 L / min for 1 hour.

[0060] 3. After the treatment was completed, pure nitrogen was switched and the flow rate was controlled at 3 L / min to continue purging for 3 hours. Then, the mixture was cooled to room temperature under nitrogen protection to obtain 1.95 kg of activated magnesium.

[0061] Example 2:

[0062] 1. Dechlorination of bis(diethylamino)silane: Add 410 kg of crude bis(diethylamino)silane with a chlorine content of 56 ppm to the evaporator, then add 46 g of activated magnesium, and then heat to 40 °C and stir for 10 hours.

[0063] 2. After the reaction is complete, the mixture is heated to 50-60℃ and subjected to vacuum distillation at a pressure below 1 kPa to obtain 400 kg of bis(diethylamino)silane.

[0064] 3. The bis(diethylamino)silane obtained after dechlorination was found to have a chlorine content of 0.95 ppm. GC-MS analysis confirmed that no hydrolysis byproducts such as siloxanes were detected.

[0065] Example 3:

[0066] 1. Dechlorination of bis(diethylamino)silane: Add 397 kg of crude bis(diethylamino)silane with a chlorine content of 60 ppm to the evaporator, then add 72 g of activated magnesium, and then heat to 40 °C and stir for 12 hours.

[0067] 2. After the reaction is complete, the mixture is heated to 50-60℃ and subjected to vacuum distillation at a pressure below 1 kPa to obtain 390 kg of bis(diethylamino)silane.

[0068] 3. The bis(diethylamino)silane obtained after dechlorination was found to have a chlorine content of 0.53 ppm. GC-MS analysis confirmed that no hydrolysis byproducts such as siloxanes were detected.

[0069] Example 4:

[0070] 1. Dechlorination of diisopropylaminosilane: Add 323 kg of crude diisopropylaminosilane with a chlorine content of 85 ppm to the evaporator, then add 110 g of activated magnesium, and then heat to 50°C and stir for 11 hours.

[0071] 2. After the reaction is complete, the mixture is heated to 50-60℃ and subjected to vacuum distillation at a pressure below 1 kPa to obtain 315 kg of diisopropylaminosilane.

[0072] 3. The diisopropylaminosilane obtained after dechlorination was found to have a chlorine content of 0.36 ppm. GC-MS analysis confirmed that no hydrolysis byproducts such as siloxanes were detected.

[0073] Example 5:

[0074] 1. Dechlorination of diisopropylaminosilane: Add 365 kg of crude diisopropylaminosilane with a chlorine content of 70 ppm to the evaporator, then add 103 g of activated magnesium, and then heat to 50 °C and stir for 12 hours.

[0075] 2. After the reaction is complete, the mixture is heated to 50-60℃ and subjected to vacuum distillation at a pressure below 1 kPa to obtain 353 kg of diisopropylaminosilane.

[0076] 3. The diisopropylaminosilane obtained after dechlorination was found to have a chlorine content of 0.23 ppm. GC-MS analysis confirmed that no hydrolysis byproducts such as siloxanes were detected.

[0077] An aminosilane purification device capable of efficiently removing chloride ions is applied to the aforementioned aminosilane purification process capable of efficiently removing chloride ions. The metal activation tower includes a tower body 1 and an activation column 2 disposed inside the tower body 1. The activation column 2 is provided with a packing component 3, which includes a rotating cylinder 31. A perforated frame 32 is fixedly connected inside the rotating cylinder 31. Multiple gas channels 33 are formed between the inner cavity of the rotating cylinder 31 and the perforated frame 32. After the gas passes through the perforated frame 32 and fully contacts the packing, it carries the impurities and is discharged from the activation column 2.

[0078] The tower body 1 is a detachable mechanism, including a top, middle and bottom, wherein the middle part can be rotated open.

[0079] Specifically, the hollow frame 32 has a fan-shaped structure and a filling chamber inside. The top and bottom of the rotating cylinder 31 are respectively fixedly connected to the feed pipe 12 and the discharge pipe 13. Magnesium shavings enter the filling chamber through the feed pipe 12. The filling ratio is 50%-75%. The hollow frame 32 has multiple evenly arranged small holes. In this embodiment, the diameter of the magnesium shavings is 0.4-0.6 cm and the inner diameter of the small holes is 0.2-0.4 cm, which can block the magnesium shavings.

[0080] In a further embodiment of the present invention, a rotating component 4 is provided inside the activation column 2, an annular groove is provided on the rotating cylinder 31, a sealing ring 41 is rotatably connected in the annular groove, an air inlet pipe 42 and an air outlet pipe 43 (both made of flexible hose or corrugated pipe material) are fixedly connected to the sealing ring 41, a reduction motor 44 is fixedly connected to the bottom of the activation column 2, the output end of the reduction motor 44 is fixedly connected to the rotating cylinder 31 located at the bottom, a telescopic component 45 is provided between adjacent rotating cylinders 31, and the reduction motor 44 drives multiple rotating cylinders 31 to rotate at a set angle through multiple transmission components.

[0081] When HCl gas enters the rotating drum 31, it comes into contact with magnesium shavings through the small hole and is discharged from the outlet pipe 43 carrying water vapor.

[0082] Optionally, a pair of baffles 35 are rotatably connected inside the rotating drum 31 to form a fixed channel through which gas flows. While reacting with magnesium shavings to remove magnesium oxide, the gas is discharged with water vapor, effectively preventing water vapor from remaining in other packing cavities.

[0083] A smooth plate 34 is fixedly connected between a pair of adjacent hollow frames 32, and the plate has a smooth structure.

[0084] A receiving plate is fixedly connected between the blocking plates 35, and a connecting rod 11 is fixedly connected between an adjacent pair of receiving plates. The connecting rod 11 moves through the rotating cylinder 31 of the accessory, so that the positions of the connecting rod 11, the receiving plate and the blocking plate 35 always remain stationary, while the positions of the rotating cylinder 31 and the connected hollow frame 32 rotate according to a set time.

[0085] In a further embodiment of the present invention, a plurality of fixing rings 5 ​​are fixedly connected inside the activation column 2, and a plurality of vibrators 6 are fixedly connected between the fixing rings 5 ​​and the rotating cylinder 31.

[0086] By setting up vibrator 6, the unactivated magnesium shavings are constantly vibrating and turning, which allows the internal magnesium shavings to react with HCl gas. The HCl gas flows slowly, allowing it to fully contact and react with the magnesium shavings, thus removing magnesium oxide from them.

[0087] The device can be set to rotate once every 10-15 minutes to control the contact time between magnesium shavings and HCl gas. This prevents excessive contact between the magnesium shavings and HCl gas, which would cause the magnesium, after magnesium oxide removal, to continue reacting with HCl gas to produce hydrogen, thus consuming magnesium and reducing the reaction yield.

[0088] In a further embodiment of the present invention, a hydraulic rod 7 is provided inside the activation column 2, the end of the hydraulic rod 7 is in contact with the inside of the activation column 2, a support rod 8 is fixedly connected to the outside of the activation column 2, and the support rod 8 is rotatably connected to the inner wall of the tower body 1. When the hydraulic rod 7 is activated, it drives the activation column 2 to tilt.

[0089] Specifically, the hydraulic cylinder 7 is fixedly connected to the inner wall of the tower body 1, and a push block is fixedly connected to the bottom of the activation column 2. The push block is movably connected to the hydraulic rod 7. The hydraulic cylinder 7 is electrically connected through the controller. When the hydraulic cylinder 7 is started, it can push the activation column 2 to rotate to an inclined angle.

[0090] Preferably, a sealing plate 9 is movably connected to the outer side of the perforated frame 32, and an electromagnet 10 is fixedly connected to the side end of the sealing plate 9. When the hydraulic rod 7 is opened, the activation column 2 begins to tilt 15-30 degrees and continues to start the vibrator 6. When the vibrator 6 is working, it vibrates and sieves the activated magnesium shavings and magnesium chloride. At this time, the electromagnets 10 on the outer side of the pair of perforated frames 32 on the right side are de-energized, so that the perforated frame 32 returns to its original position under the action of elasticity, sealing the small hole on the outer side of the perforated frame 32 on the right side. The magnesium chloride falls to the outside of the perforated frame 32 on the left side and does not fall into the inside of the perforated frame 32 on the right side. At this time, the inert gas (nitrogen and argon) has a large flow rate (3-5L / min), which can blow out the magnesium chloride along with the other gases (residual HCl gas, trace water vapor and trace hydrogen gas), thereby achieving the purpose of effectively removing magnesium chloride powder.

[0091] The sealing plate 9 has a chamfer and a smooth arc surface structure at the outer end.

[0092] In this invention, when entering the purification stage, it is necessary to remove the impurities from the previous reaction. Since magnesium chloride is solid and mixed in magnesium shavings, it needs to be vibrated and sieved. During the sieving process, magnesium chloride falls into the gas channel and is discharged from the tower 1 along with the inert gas.

[0093] The outer end of the rotating drum 31 is provided with a feed pipe 12 (which adopts a corrugated pipe structure and is connected to the movable ring 41). When the activation column 2 is tilted, the feed pipe 12 is stretched. Adjacent pairs of rotating drums 31 are fixedly connected by a telescopic member 45. The telescopic member 45 (which can be a telescopic tube) is hollow inside and is equipped with a solenoid valve. The discharge pipe 13 is provided below the bottom rotating drum 31, and the bottom of the tower body 1 is provided with a discharge pipe 14. When activated magnesium needs to be removed, the solenoid valve can be controlled to remove all the activated magnesium.

[0094] The foregoing has only described certain exemplary embodiments of the present invention by way of illustration. Undoubtedly, those skilled in the art can modify the described embodiments in various ways without departing from the spirit and scope of the present invention. Therefore, the foregoing drawings and descriptions are illustrative in nature and should not be construed as limiting the scope of protection of the claims of the present invention.

Claims

1. A process for purifying amino silane with high removal of chloride ions, comprising a metal activation column, characterized in that: The steps are as follows, S1: activation column filling: the unactivated magnesium chips are uniformly filled in the activation column in the metal activation tower, and the system is placed in an inert gas state by replacing with inert gas; S2: HCl gas activation and film removal: the activation column is heated to 200 DEG C, and pure HCl gas with a purity of 99.9% is introduced into the activation column, and the activation reaction is maintained for 1h, and the water generated by the reaction of HCl gas and magnesium oxide on the surface of magnesium is discharged in gaseous form with tail gas; S3: activation stage opens the vibrator, and controls the rotation of the activation column every set time to rotate by a set angle, so that the HCl gas is uniformly reacted with the unactivated magnesium chips; S4: magnesium purification after activation: stop introducing HCl gas, and introduce inert gas into the activation column for 3h, and the blowing temperature is maintained at 200 DEG C, and the residual HCl gas, trace gaseous water and trace magnesium chloride are removed; S5: purification stage, control the rotation of the movable cylinder to the inclined position, open the vibrator, and the powdered magnesium chloride is shaken off, and then is blown out of the activation column by inert gas; S6: then cooled to room temperature under argon protection, and in the process of cooling to room temperature, the argon flow is reduced to 0.2-0.4 L / min, and finally the activated magnesium is obtained; S7: under the conditions of anhydrous and anaerobic, the amino silane raw material containing chloride ions is mixed with the above activated magnesium, and then heated and stirred for 10-12 hours, and after the reaction is completed, vacuum distillation is carried out, and low-chlorine amino silane is obtained.

2. The amino-silane purification process capable of efficiently removing chloride ions according to claim 1, characterized in that, The flow rate of the HCl gas is controlled at 0.5 L / min, and the flow rate of the inert gas is controlled at 3 L / min.

3. The amino-silane purification process capable of efficiently removing chloride ions according to claim 1, characterized in that, The hydrogen chloride gas in S2 is introduced after being diluted with inert gas, and the dilution concentration is 5-20 vol%.

4. The amino-silane purification process capable of efficiently removing chloride ions according to claim 1, characterized in that, The amount of the activated magnesium is 2-4:1 molar ratio of the chlorine atom in the amino silane raw material.

5. The amino-silane purification process capable of efficiently removing chloride ions according to claim 1, characterized in that, The heating temperature in S7 is 40-50 DEG C.

6. The amino-silane purification process capable of efficiently removing chloride ions according to claim 5, characterized in that, The temperature of the vacuum distillation is 50-60 DEG C, and the vacuum degree is below 1 kPa.

7. The amino-silane purification device capable of efficiently removing chloride ions, applied to the amino-silane purification process capable of efficiently removing chloride ions according to any one of claims 1-6, characterized in that, The metal activation tower comprises a tower body and an activation column arranged in the tower body, the activation column is provided with a filler component, the filler component comprises a rotating drum, the inside of the rotating drum is fixedly connected with a hollow frame, a plurality of gas cavities are formed between the inner cavity of the rotating drum and the hollow frame, and the gas is discharged out of the activation column after fully contacting with the filler through the hollow frame.

8. The amino-silane purification device capable of efficiently removing chloride ions according to claim 7, characterized by, The activation column is also provided with a rotating component, an annular groove is formed in the rotating drum, the annular groove is rotatably connected with a sealing ring, the sealing ring is fixedly connected with a gas inlet pipe and a gas outlet pipe, the bottom of the activation column is fixedly connected with a speed reducer, the output end of the speed reducer is fixedly connected with the lowermost rotating drum, a telescopic member is arranged between adjacent rotating drums, and the speed reducer drives a plurality of rotating drums to rotate by a plurality of transmission members.

9. The amino-silane purification device capable of efficiently removing chloride ions according to claim 8, characterized by, A plurality of fixed rings are fixedly connected in the activation column, and a plurality of vibrators are fixedly connected between the rotating drums.

10. The amino-silane purification device capable of efficiently removing chloride ions according to claim 9, characterized by, A hydraulic rod is arranged in the activation column, the end of the hydraulic rod is abuttingly connected with the activation column, a support rod is fixedly connected outside the activation column, the support rod is rotatably connected with the inner wall of the tower body, and the activation column is driven to be in an inclined state when the hydraulic rod is started.

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