A method for purifying trimethylsilane

By using the reaction and distillation techniques of magnesium scrap and crude trimethylsilane, the problem of removing impurities from trimethylsilane has been solved, achieving efficient and low-cost purification of trimethylsilane and improving the performance and stability of electronic components.

CN120590433BActive Publication Date: 2025-11-14ANHUI ARGOSUN NEW ELECTRONIC MATERIALS CO LTD
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Patent Information

Application Number
CN202510744242.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-06-05
Publication Date
2025-11-14
Estimated Expiration
2045-06-05

AI Technical Summary

Technical Problem

Existing technologies are insufficient to effectively remove chlorinated organic impurities and trace amounts of dimethylsilane from crude trimethylsilane, leading to performance degradation or failure of electronic components.

Method used

Under inert gas protection, magnesium filings are reacted with crude trimethylsilane. Combined with a fractionation unit and distillation technology, the magnesium filings react with chlorine-containing organic matter, and the fractionation unit prevents the magnesium filings from precipitating. Subsequently, distillation is carried out to remove light components, thereby purifying trimethylsilane.

Benefits of technology

The production of high-purity trimethylsilane has been achieved at a low cost and with less complexity, improving reaction efficiency and purity to meet the needs of semiconductor and integrated circuit manufacturing.

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Abstract

This invention discloses a method for purifying trimethylsilane, comprising the following steps: S1: Magnesium shavings are added to a reaction vessel under an inert gas environment, the reaction vessel temperature is controlled at -10~0℃, and crude trimethylsilane containing chlorine is added to the reaction vessel. Stirring is started, and the condenser temperature is -30~-20℃; S2: The reaction vessel pressure is controlled at 300KPa, the temperature at 30~35℃, and stirring is performed for 6 hours; S3: After stirring, the pressure is restored to normal to distill off the trimethylsilane, which is collected in a crude product receiving tank and finally transferred to a refined product receiving tank. In the distillation vessel; S4: Control the pressure of the distillation vessel to 200 kPa and the temperature to 25-30°C for distillation, and remove light components at a ratio of 5-8%; S5: Receive the fraction at about 25°C and collect it in the receiving tank to complete the purification of trimethylsilane. The reactor also includes a classification component, which is used to classify the magnesium shavings in step S1. The classification component includes multiple support cylinders, which are slidably connected and abutting each other. Each support cylinder is equipped with an anti-settling component to prevent magnesium shavings from settling at the bottom of the support cylinder.
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Description

Technical Field

[0001] This invention relates to the field of trimethylsilane production technology, and more specifically to a method for purifying trimethylsilane. Background Technology

[0002] Trimethylsilane ((CH3)3SiH), as an important organosilicon compound, has wide applications in the semiconductor and integrated circuit fields.

[0003] In semiconductor manufacturing, trimethylsilane is frequently used as a precursor in chemical vapor deposition (CVD) processes. Through CVD, it can deposit thin films on semiconductor wafers, which are widely used to fabricate insulating, dielectric, conductive, or other functional layers. Furthermore, trimethylsilane can be used to prepare low-k materials, which help reduce capacitance during signal transmission in semiconductor devices, thereby reducing circuit delay and power consumption—crucial for advanced semiconductor processes.

[0004] Trimethylsilane also plays an indispensable role in integrated circuit manufacturing. It is not only an important precursor for depositing silicon-containing thin films, but is also used in various deposition processes, such as plasma-enhanced chemical vapor deposition (PECVD) and atomic layer deposition (ALD). These processes can precisely control the thickness and composition of the thin film, thereby meeting the demands of integrated circuits for high performance and miniaturization. Especially in the fabrication of interconnect layers, dielectric layers, and passivation layers, trimethylsilane-deposited films play a crucial role in connecting transistors, preventing current leakage, and protecting the chip from environmental influences.

[0005] Crude trimethylsilane contains some low-boiling-point impurities, such as chlorinated organic compounds and dimethylsilane. In the current technology, it is difficult to completely remove these chlorinated organic impurities and trace amounts of dimethylsilane when purifying crude trimethylsilane. These impurities can easily lead to a decrease in the performance of electronic components prepared from it or even failure. Summary of the Invention

[0006] The purpose of this invention is to provide a method for purifying trimethylsilane to overcome the aforementioned shortcomings in the prior art.

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

[0008] A method for purifying trimethylsilane includes the following steps:

[0009] S1: Add magnesium shavings to the reactor under an inert gas environment, control the reactor temperature to -20~0℃, add crude trimethylsilane containing chlorine to the reactor, start stirring, and keep the condenser temperature at -30~-20℃;

[0010] S2: Control the reactor pressure at 300 kPa, the temperature at 30~35℃, and stir for 6 hours;

[0011] S3: After stirring, restore atmospheric pressure to distill off trimethylsilane, collect it in the crude product receiving tank, and finally transfer it to the bottom of the distillation vessel;

[0012] S4: Control the pressure of the bottom distillation vessel at 200 kPa and the temperature at 25-30℃ to carry out distillation, removing light components at a ratio of 5-8%;

[0013] S5: Receive the fraction at around 25°C and collect it in the receiving tank to complete the purification of trimethylsilane;

[0014] The reactor also includes a grading component for grading the magnesium shavings in step S1. The grading component includes multiple support cylinders, which are slidably connected and abut against each other. Each support cylinder is provided with an anti-settling component to prevent magnesium shavings from settling at the bottom of the support cylinder.

[0015] Preferably, steps S1 to S5 are all performed under inert gas protection, and the water and oxygen content of the inert gas is less than 1 ppm.

[0016] Preferably, in step S1, the amount of magnesium shavings is 1.5 to 4 times the chloride ion content.

[0017] Preferably, the anti-sinking component includes a lifting seat, which is fitted to the bearing cylinder, and a plurality of anti-sinking plates are fixedly arranged on the lifting seat, each of the anti-sinking plates being provided with a plurality of material through holes;

[0018] Each of the aforementioned anti-sinking plates is fixedly equipped with a protective plate.

[0019] Preferably, a rotating frame is rotatably mounted on the bearing cylinder, and the rotating frame is slidably connected to the lifting seat;

[0020] Multiple springs are provided between the lifting seat and the bearing cylinder, and the two ends of the multiple springs are fixedly connected to the lifting seat and the bearing cylinder respectively.

[0021] Preferably, a stirring shaft is rotatably mounted on the reactor, an abutment pin is fixedly mounted on the lifting seat, and an abutment rod is fixedly mounted on the stirring shaft, the abutment rod being adapted to the abutment pin;

[0022] Both the abutment rod and the abutment pin are provided with bevels.

[0023] Preferably, it also includes a reciprocating lead screw, which is provided with a sliding groove, and a fixing block is provided on the bearing cylinder located at the bottom, the fixing block being slidably disposed in the sliding groove;

[0024] Furthermore, the support cylinder located at the bottom is slidably connected to the reactor, while the support cylinder located at the top is fixedly connected to the reactor;

[0025] The reciprocating lead screw abuts against the lifting seat located on the lowest bearing cylinder.

[0026] Preferably, a first pulley and a second pulley are rotatably mounted on the reactor. The first pulley is threadedly connected to a reciprocating lead screw, and a belt is provided between the first pulley and the second pulley for transmission.

[0027] Preferably, a ratchet block is rotatably mounted on the stirring shaft, a ratchet ring is fixedly mounted on the second pulley, the ratchet block and the ratchet ring are engaged, and a torsion spring is provided between the ratchet block and the stirring shaft.

[0028] The purification method for trimethylsilane provided by the present invention, as described above, has the following beneficial effects:

[0029] 1. The method involves removing chlorine-containing organic impurities from crude trimethylsilane by reacting magnesium shavings with the trimethylsilane, then distilling off the trimethylsilane and removing light components such as dimethylsilane by fractional distillation. This process achieves purification of trimethylsilane. Testing has shown that this method is low-cost, produces high-purity trimethylsilane, and is relatively simple.

[0030] 2. In the reaction process of crude trimethylsilane containing chlorine and magnesium filings, by feeding the magnesium filings into multiple support cylinders and positioning the support cylinders at different heights during the reaction, the magnesium filings are prevented from settling at the bottom of the reactor, which would lead to incomplete reaction and excessive stirring time. At the same time, by setting anti-settling components, the accumulation of magnesium filings in the reactor is prevented, thereby reducing the contact area between the magnesium filings and the crude trimethylsilane containing chlorine and effectively improving the reaction efficiency.

[0031] 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.

[0032] 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

[0033] 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.

[0034] Figure 1This is a schematic diagram of the internal structure of the reaction vessel provided in an embodiment of the present invention;

[0035] Figure 2 These are schematic diagrams of various bearing cylinder structures provided in embodiments of the present invention;

[0036] Figure 3 Provided for embodiments of the present invention Figure 2 Enlarged view of point A in the image;

[0037] Figure 4 Provided for embodiments of the present invention Figure 2 Enlarged view of point B in the image;

[0038] Figure 5 This is a schematic diagram of the anti-sinking component structure provided in an embodiment of the present invention;

[0039] Figure 6 This is a schematic diagram of the transmission structure of the first pulley and the second pulley provided in an embodiment of the present invention.

[0040] Explanation of reference numerals in the attached figures:

[0041] 1. Reactor; 11. Stirring shaft; 12. Ratchet block; 13. Feed inlet; 14. Motor; 2. Bearing cylinder; 21. Fixing block; 3. Rotating frame; 31. Spring; 4. Lifting seat; 41. Anti-sinking plate; 42. Protective plate; 43. Material through hole; 44. Abutment pin; 5. Reciprocating screw; 51. Sliding groove; 6. First pulley; 61. Belt; 7. Second pulley; 71. Ratchet ring; 8. Abutment rod. Detailed Implementation

[0042] 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.

[0043] Please refer to 1-6, a method for purifying trimethylsilane, comprising the following steps:

[0044] S1: Magnesium shavings are added to reactor 1 under an inert gas environment, the temperature of reactor 1 is controlled at -20~0℃, and crude trimethylsilane containing chlorine is added to reactor 1. Stirring is started, and the temperature of the condenser is -30~-20℃.

[0045] S2: Control the pressure of reactor 1 at 300 kPa and the temperature at 30~35℃, and stir for 6 hours;

[0046] S3: After stirring, restore atmospheric pressure to distill off trimethylsilane, collect it in the crude product receiving tank, and finally transfer it to the bottom of the distillation vessel;

[0047] S4: Control the pressure of the bottom distillation vessel at 200 kPa and the temperature at 25-30℃ to carry out distillation, removing light components at a ratio of 5-8%;

[0048] S5: Receive the fraction at around 25°C and collect it in the receiving tank to complete the purification of trimethylsilane;

[0049] The reactor 1 also includes a grading component, which is used to grade the magnesium shavings in step S1. The grading component includes multiple support cylinders 2, which are slidably connected and abut against each other. Each support cylinder 2 is provided with an anti-settling component to prevent magnesium shavings from settling at the bottom of the support cylinder 2.

[0050] S1 to S4 were all carried out under inert gas protection, and the water and oxygen content of the inert gas was less than 1 ppm.

[0051] The amount of magnesium shavings is 1.5 to 4 times the chloride ion content.

[0052] Example 1

[0053] 1. 300 kg of crude trimethylsilane to be transferred was sampled and tested. The chloride ion content was found to be 5000 ppm, which is approximately 717.1 g (20.2 mol).

[0054] 2. Under inert gas protection, transfer 0.73 kg of magnesium shavings to the reactor for purging (total value of other gases and water < 1 ppm), control the reactor temperature to -10~0℃, then transfer 300 kg of crude trimethylsilane (containing chlorine) to the reactor, start stirring, and control the condenser temperature to -30~-20℃.

[0055] 3. Control the pressure of the reactor to 300 kPa and the temperature to 30°C, stir for 6 hours, and after stirring, restore the pressure to normal pressure to distill off the trimethylsilane, collect it in the crude product receiving tank, and finally transfer it to the bottom of the distillation vessel.

[0056] 4. Distill at a pressure of 200 kPa and a temperature of 25-30°C in the bottom distillation vessel. Remove light components at a ratio of 5%, and then collect 247.8 kg of the fraction at around 25°C into the product tank, which is the finished trimethylsilane product.

[0057] In this case, the trimethylsilane purification yield was 82.6%. The product was tested by IC, GC and ICP and all inorganic elements were <1ppm, of which chlorine was <0.7ppm, and the purity reached 6N.

[0058] Example 2

[0059] 1. The 308 kg of crude trimethylsilane to be transferred was sampled and tested. The chloride ion content was 8032 ppm, which means the chloride ion content was approximately 1182.2 g (33.3 mol).

[0060] 2. Under inert gas protection, transfer 2.4 kg of magnesium shavings to the reactor for purging (total value of other gases and water < 1 ppm), control the reactor temperature to -10~0℃, then transfer 308 kg of crude trimethylsilane (containing chlorine) to the reactor, start stirring, and control the condenser temperature to -30~-20℃.

[0061] 3. Control the pressure of the reactor to 300 kPa and the temperature to 30°C, stir for 6 hours, and after stirring, restore the pressure to normal pressure to distill off the trimethylsilane, collect it in the crude product receiving tank, and finally transfer it to the bottom of the distillation vessel.

[0062] 4. Distill at a pressure of 200 kPa and a temperature of 25-30°C in the bottom distillation vessel. Remove light components at a ratio of 8%, and then collect 251 kg of the fraction at around 25°C in the product tank, which is the trimethylsilane product.

[0063] In this case, the trimethylsilane purification yield was 81.5%. The product was tested by IC, GC and ICP and all inorganic elements were <1ppm, with chlorine <0.5ppm, and the purity reached 6N.

[0064] Example 3

[0065] 1. The 312 kg of crude trimethylsilane to be transferred was sampled and tested. The chloride ion content was found to be 6256 ppm, which means the chloride ion content was approximately 933.7 g (26.3 mol).

[0066] 2. Under inert gas protection, transfer 1.26 kg of magnesium shavings to the reactor for purging (total value of other gases and water < 1 ppm), control the reactor temperature to -10~0℃, then transfer 312 kg of crude trimethylsilane (containing chlorine) to the reactor, start stirring, and control the condenser temperature to -30~-20℃.

[0067] 3. Control the pressure of the reactor to 300 kPa and the temperature to 30°C, stir for 6 hours, and after stirring, restore the pressure to normal pressure to distill off the trimethylsilane, collect it in the crude product receiving tank, and finally transfer it to the bottom of the distillation vessel.

[0068] 4. Distill at a pressure of 200 kPa and a temperature of 25-30°C in the bottom distillation vessel. Remove light components at a ratio of 6%, and then collect 256.2 kg of the fraction at around 25°C into the product tank, which is the trimethylsilane product.

[0069] In this case, the trimethylsilane purification yield was 82.1%. The product was tested by IC, GC and ICP and all inorganic elements were <1ppm, of which chlorine was <0.6ppm, and the purity reached 6N.

[0070] In the reaction of crude trimethylsilane containing chlorine with magnesium filings, by feeding the magnesium filings into multiple support cylinders 2 and positioning the support cylinders 2 at different heights during the reaction, the magnesium filings are prevented from settling at the bottom of the reactor 1, thus preventing incomplete reaction and excessive stirring time. At the same time, by setting anti-settling components, the accumulation of magnesium filings in the reactor 1 is prevented, thereby reducing the contact area between the magnesium filings and the crude trimethylsilane containing chlorine, effectively improving the reaction efficiency.

[0071] Specifically, the anti-settling component includes a lifting seat 4, which is attached to the bearing cylinder 2. Multiple anti-settling plates 41 are fixedly installed on the lifting seat 4, and each anti-settling plate 41 has multiple material penetration holes 43. A protective plate 42 is fixedly installed on each anti-settling plate 41. During the reaction of the chlorinated trimethylsilane crude product with magnesium shavings, the motor 14 drives the stirring shaft 11 to make the lifting seat 4 rotate synchronously. The rotation of the lifting seat 4 and the anti-settling plates 41 prevents magnesium shavings from settling on the lifting seat 4 and allows the magnesium shavings to be lifted and pass through... The material passage 43 prevents magnesium shavings from adhering to the anti-settling plate 41, increasing the contact area between the crude chlorinated trimethylsilane and the magnesium shavings, thereby increasing the reaction rate. Furthermore, a protective plate 42 is installed on the anti-settling plate 41 to prevent the magnesium shavings, which are thrown up by the anti-settling plate 41, from escaping from the support cylinder 2 and settling at the bottom of the reactor 1. During the reaction, multiple support cylinders 2 are located at different heights inside the reactor 1, which can further enhance the reaction effect between the crude chlorinated trimethylsilane and the magnesium shavings and avoid incomplete reaction.

[0072] In a further embodiment of the present invention, a rotating frame 3 is rotatably mounted on the support cylinder 2, and the rotating frame 3 is slidably connected to the lifting seat 4; a plurality of springs 31 are provided between the lifting seat 4 and the support cylinder 2, and the two ends of the plurality of springs 31 are fixedly connected to the lifting seat 4 and the support cylinder 2 respectively. During the reaction, the rotating frame 3 and the lifting seat 4 rotate synchronously to improve the stability of the lifting seat 4 during the rotation process. After the reaction is completed, the lifting seat 4 is lowered, the springs 31 are stretched, and the lifting seat 4 is separated from the support cylinder 2. Since the contact surface between the lifting seat 4 and the support cylinder 2 is set at an incline, the by-products or unreacted magnesium shavings generated inside the support cylinder 2 can be discharged and precipitated to the bottom of the reaction vessel 1.

[0073] Furthermore, a stirring shaft 11 is rotatably mounted on the reactor 1, and an abutment pin 44 is fixedly mounted on the lifting seat 4. An abutment rod 8 is fixedly mounted on the stirring shaft 11, and the abutment rod 8 is adapted to the abutment pin 44. Both the abutment rod 8 and the abutment pin 44 are provided with inclined surfaces. When magnesium shavings are put into each of the bearing cylinders 2, each bearing cylinder 2 slides down to different heights. The abutment pin 44 on the lifting seat 4 of each bearing cylinder 2 also moves down to the corresponding position of the abutment rod 8. The stirring shaft 11 rotates, and the stirring blades on the stirring shaft 11 stir the mixture. At the same time, the abutment rod 8 rotates and interacts with the corresponding abutment pin 44 during the rotation. 4. After contact, the lifting seat 4 rotates via the contact pin 44, causing the lifting seat 4 and the rotating frame 3 to rotate. The anti-sinking plate 41 prevents magnesium shavings from settling at the bottom of the bearing cylinder 2. By setting inclined surfaces on the contact pin 44 and the contact rod 8, if the contact pin 44 and the contact rod 8 are at the same angle during the descent of the bearing cylinder 2 and a collision occurs, the mutual squeezing of the inclined surfaces can prevent the descent of the bearing cylinder 2 from being restricted. When the contact rod 8 rotates, it contacts the upper part of the inclined surface on the contact pin 44, thereby pushing the lifting seat 4 to rotate and improving the rotational stability of the lifting seat 4.

[0074] Furthermore, it also includes a reciprocating screw 5, which is equipped with a sliding groove 51. A fixing block 21 is provided on the lowest bearing cylinder 2, and the fixing block 21 is slidably disposed in the sliding groove 51. The lowest bearing cylinder 2 is slidably connected to the reactor 1, and the uppermost bearing cylinder 2 is fixedly connected to the reactor 1. The reciprocating screw 5 abuts against the lifting seat 4 on the lowest bearing cylinder 2. When magnesium chips are added, all bearing cylinders 2 are at the same height at the top. After the magnesium chips are added into each bearing cylinder 2, the reciprocating screw 5 moves the lowest bearing cylinder 2 downward. At this time, under the action of gravity, all bearing cylinders 2 except the uppermost bearing cylinder 2 move downward. Since the uppermost bearing cylinder 2 is fixedly connected to the reactor 1, when each bearing cylinder 2 moves downward, the bearing cylinder... When the lifting seat 4 of the upper support cylinder 2 comes into contact with the upper support cylinder 2, it is restricted from moving downward by the force of the spring 31, so that each support cylinder 2 stops at a different height. After the reaction is completed, the reciprocating screw 5 continues to move downward, pressing down on the lower support cylinder 2, causing the adjacent lifting seat 4 to move downward. The spring 31 is stretched, and after stretching, while the lower support cylinder 2 continues to move downward, each support cylinder 2 moves downward with the lifting seat 4 on the adjacent support cylinder 2. In this way, the lifting seat 4 on each support cylinder 2 is separated from the corresponding support cylinder 2, so that the reaction by-products or unreacted magnesium shavings in the support cylinder 2 are precipitated out from the support cylinder 2 and accumulate at the bottom outlet of the reactor 1, so as to facilitate the cleaning of the products inside the reactor 1 after the reaction.

[0075] As the support cylinder 2 rises, the reciprocating screw 5 moves the bottom support cylinder 2 upwards. When it reaches the same height as the adjacent support cylinder 2, it comes into contact with the adjacent support cylinder 2 and moves it upwards. In this way, the reciprocating screw 5 moves each support cylinder 2 to the feed inlet 13 position at the top of the reactor 1. The shape and size of the feed inlet 13 can be adjusted according to the actual application to make it easier to put magnesium shavings into each support cylinder 2.

[0076] In a further embodiment of the present invention, a first pulley 6 and a second pulley 7 are rotatably arranged on the reactor 1. The first pulley 6 is threadedly connected to the reciprocating screw 5, and a belt 61 is provided between the first pulley 6 and the second pulley 7 for transmission. The rotation of the second pulley 7 drives the first pulley 6 to rotate through the belt 61, thereby realizing the up and down movement of the reciprocating screw 5. The second pulley 7 only needs to rotate in one direction to complete the rise and fall of the reciprocating screw 5, thereby completing the rise and fall of the bearing cylinder 2.

[0077] When each bearing cylinder 2 is lowered to the reaction height, the top of the reciprocating screw 5 does not descend to contact the first pulley 6. After the reaction is completed, the first pulley 6 continues to rotate, causing the reciprocating screw 5 to continue to move downward, completing the separation of each bearing cylinder 2 from the corresponding lifting seat 4. When the product inside the bearing cylinder 2 precipitates out, the top of the reciprocating screw 5 contacts the first pulley 6. After the product inside the bearing cylinder 2 precipitates out, the first pulley 6 continues to rotate. Under the characteristics of the reciprocating screw 5, the reciprocating screw 5 rises, causing each bearing cylinder 2 to rise to the feeding position.

[0078] In the embodiment provided by the present invention, a ratchet block 12 is rotatably mounted on the stirring shaft 11, and a ratchet ring 71 is fixedly mounted on the second pulley 7. The ratchet block 12 and the ratchet ring 71 are engaged. A torsion spring is provided between the ratchet block 12 and the stirring shaft 11. By setting the ratchet block 12 and the ratchet ring 71, the motor 14 drives the stirring shaft 11 to rotate. The engagement of the ratchet block 12 and the ratchet ring 71 enables transmission between the first pulley 6, the belt 61, and the second pulley 7, thereby realizing the lifting and lowering of the reciprocating screw 5. After the reciprocating screw 5 has lifted and lowered, the motor 14 drives the stirring shaft 11 to reverse and carry out the stirring reaction. Under the action of the ratchet block 12 and the torsion spring, the ratchet block 12 does not drive the ratchet ring 71 to rotate. Therefore, the first pulley 6 and the second pulley 7 will not rotate, keeping the reciprocating screw 5 stable and maintaining the stability of each bearing cylinder 2.

[0079] 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 method for purifying trimethylsilane, characterized in that, Includes the following steps: S1: Magnesium shavings are added to the reactor (1) under an inert gas environment. The temperature of the reactor (1) is controlled at -10~0℃. Chlorine-containing crude trimethylsilane is added to the reactor (1). Stirring is started. The temperature of the condenser is -30~-20℃. S2: Control the reactor pressure at 300 kPa, the temperature at 30~35℃, and stir for 6 hours; S3: After stirring, restore atmospheric pressure to distill off trimethylsilane, collect it in the crude product receiving tank, and finally transfer it to the bottom of the distillation vessel; S4: Control the pressure of the bottom distillation vessel at 200 kPa and the temperature at 25~30℃ to carry out distillation and remove light components at a ratio of 5~8%; S5: Receive the fraction at 25℃ and collect it in the receiving tank to complete the purification of trimethylsilane; The reactor (1) also includes a grading component for grading the magnesium shavings in step S1. The grading component includes multiple support cylinders (2), each of which is slidably connected and abutting against each other. Each of the support cylinders (2) is provided with an anti-settling component to prevent magnesium shavings from settling at the bottom of the support cylinder (2).

2. The method for purifying trimethylsilane according to claim 1, characterized in that, S1 to S5 are all carried out under inert gas protection, and the water and oxygen content of the inert gas is less than 1 ppm.

3. The method for purifying trimethylsilane according to claim 1, characterized in that, In S1, the amount of magnesium shavings is 1.5 to 4 times the chloride ion content.

4. The method for purifying trimethylsilane according to claim 1, characterized in that, The anti-sinking component includes a lifting seat (4), which is in contact with the bearing cylinder (2). Multiple anti-sinking plates (41) are fixedly provided on the lifting seat (4), and each anti-sinking plate (41) is provided with multiple material through holes (43). Each of the aforementioned anti-sinking plates (41) is fixedly provided with a protective plate (42).

5. The method for purifying trimethylsilane according to claim 4, characterized in that, A rotating frame (3) is rotatably mounted on the bearing cylinder (2), and the rotating frame (3) is slidably connected to the lifting seat (4); Multiple springs (31) are provided between the lifting seat (4) and the bearing cylinder (2), and the two ends of the multiple springs (31) are fixedly connected to the lifting seat (4) and the bearing cylinder (2) respectively.

6. The method for purifying trimethylsilane according to claim 4, characterized in that, The reactor (1) is rotatably equipped with a stirring shaft (11), the lifting seat (4) is fixedly equipped with an abutment pin (44), and the stirring shaft (11) is fixedly equipped with an abutment rod (8), which is adapted to the abutment pin (44). Both the abutment rod (8) and the abutment pin (44) are provided with inclined surfaces.

7. The method for purifying trimethylsilane according to claim 6, characterized in that, It also includes a reciprocating lead screw (5), on which a sliding groove (51) is provided, and a fixing block (21) is provided on the bearing cylinder (2) located at the bottom, and the fixing block (21) is slidably disposed in the sliding groove (51); The lowermost support cylinder (2) is slidably connected to the reactor (1), and the uppermost support cylinder (2) is fixedly connected to the reactor (1). The reciprocating screw (5) abuts against the lifting seat (4) on the lowermost bearing cylinder (2).

8. The method for purifying trimethylsilane according to claim 7, characterized in that, The reactor (1) is rotatably provided with a first pulley (6) and a second pulley (7). The first pulley (6) is threadedly connected to the reciprocating screw (5), and a belt (61) is provided between the first pulley (6) and the second pulley (7).

9. The method for purifying trimethylsilane according to claim 8, characterized in that, A ratchet block (12) is rotatably mounted on the stirring shaft (11), and a ratchet ring (71) is fixedly mounted on the second pulley (7). The ratchet block (12) and the ratchet ring (71) are engaged. A torsion spring is provided between the ratchet block (12) and the stirring shaft (11).

Citation Information

Patent Citations

  • Preparation process of high-purity tetramethylsilane

    CN117069756A

  • System and method for purifying trimethylsilane containing dichlorosilane impurity

    CN119565185A