Method for purifying trimethylsilane

Through the reaction and distillation technology of magnesium chips and crude trimethylsilane, the problem of incomplete impurity removal in the existing technology is solved, and the production of high-purity trimethylsilane is achieved, which is suitable for the semiconductor and integrated circuit fields.

CN120590433AActive Publication Date: 2025-09-05ANHUI ARGOSUN NEW ELECTRONIC MATERIALS CO LTD
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Patent Information

Application Number
CN202510744242.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-05
Publication Date
2025-09-05
Estimated Expiration
2045-06-05

AI Technical Summary

Technical Problem

Existing technologies make it difficult to effectively remove chlorine-containing organic impurities and trace amounts of dimethylsilane from crude trimethylsilane, which leads to performance degradation or failure of electronic components.

Method used

Magnesium chips are reacted with crude trimethylsilane in an inert gas environment. Combined with grading components and distillation technology, the purification of trimethylsilane is achieved through the reaction of magnesium chips with chlorine-containing impurities and the removal of light components by distillation.

Benefits of technology

This enables the production of high-purity trimethylsilane at low cost and with less complexity, improving reaction efficiency and purity to meet the high-performance demands of semiconductors and integrated circuits.

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Abstract

The invention discloses a purification method of trimethylsilane, which comprises the following steps: S1, adding magnesium chips into a reaction kettle in an inert gas environment, controlling the temperature of the reaction kettle to be-10 to 0 DEG C, adding a chlorine-containing trimethylsilane crude product into the reaction kettle, starting stirring, and controlling the temperature of a condenser to be-30 to-20 DEG C; s2, controlling the pressure of the reaction kettle to be 300KPa and the temperature to be 30-35 DEG C, and stirring for 6 hours; s3, after stirring is finished, normal pressure is recovered, trimethylsilane is evaporated out, and trimethylsilane is collected into a crude product receiving tank and finally transferred into a rectification bottom kettle; s4, controlling the pressure of a rectification bottom kettle to be 200KPa, controlling the temperature to be 25-30 DEG C, carrying out rectification, and removing light components according to the proportion of 5-8%; s5, fractions at the temperature of about 25 DEG C are received and collected into a receiving tank, and purification of trimethylsilane is completed. The reaction kettle further comprises a grading assembly used for grading the magnesium chips in the step S1, the grading assembly comprises a plurality of bearing cylinders, the bearing cylinders are in sliding connection and abut against each other in a matched mode, and each bearing cylinder is provided with an anti-settling part. Magnesium chips are prevented from precipitating at the bottom of the bearing cylinder.
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Description

Technical Field

[0001] The present invention relates to the technical field of trimethylsilane production, and in particular to a method for purifying trimethylsilane. Background Art

[0002] Trimethylsilane ((CH3)3SiH), as an important organosilicon compound, has a wide range of applications in the fields of semiconductors and integrated circuits.

[0003] In semiconductor manufacturing, trimethylsilane is often used as a precursor in chemical vapor deposition (CVD) processes. Through the CVD process, it can deposit thin films on semiconductor wafers. These films are widely used to manufacture insulating layers, dielectric layers, conductive layers, or other functional films. In addition, trimethylsilane can also be used to prepare low-dielectric constant (Low-k) materials. These materials help reduce the capacitance during signal transmission in semiconductor devices, thereby reducing circuit delays and power consumption, which is critical for advanced semiconductor processes.

[0004] Trimethylsilane also plays an indispensable role in integrated circuit manufacturing. It's not only a crucial precursor for depositing silicon-containing thin films, but is also used in a variety of deposition processes, such as plasma-enhanced chemical vapor deposition (PECVD) and atomic layer deposition (ALD). These processes enable precise control of film thickness and composition, thus meeting the demands of integrated circuits for high performance and miniaturization. In particular, when fabricating interconnect, dielectric, and passivation layers, thin films deposited with trimethylsilane play a crucial role in connecting transistors, preventing current leakage, and protecting chips from environmental influences.

[0005] Crude trimethylsilane contains some low-boiling-point impurities, such as chlorine-containing organic matter and dimethylsilane. In the existing technology, it is difficult to completely remove these chlorine-containing organic impurities and trace amounts of dimethylsilane when purifying crude trimethylsilane. These impurities can easily cause the performance of electronic components prepared therefrom to deteriorate or even fail. Summary of the Invention

[0006] The object of the present invention is to provide a method for purifying trimethylsilane to solve the above-mentioned deficiencies in the prior art.

[0007] In order to achieve the above object, the present invention provides the following technical solutions:

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

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

[0010] S2: Control the reactor pressure to 300 kPa, the temperature to 30-35 °C, and stir for 6 h;

[0011] S3: After the stirring is completed, the normal pressure is restored to evaporate the trimethylsilane, which is collected in a crude product receiving tank and finally transferred to the distillation bottom kettle;

[0012] S4: Control the distillation bottom kettle pressure to 200KPa and the temperature to 25~30℃ for distillation, and remove light components at a ratio of 5~8%;

[0013] S5: receiving the fraction at about 25°C and collecting it into a receiving tank to complete the purification of trimethylsilane;

[0014] The reactor also includes a grading assembly, which is used to grade the magnesium chips in step S1. The grading assembly includes a plurality of supporting tubes, each of which is slidably connected and abutted. Each of the supporting tubes is provided with an anti-sinking part to prevent the magnesium chips from settling at the bottom of the supporting tube.

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

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

[0017] Preferably, the anti-sinking member comprises a lifting seat, the lifting seat is fitted with the carrying cylinder, a plurality of anti-sinking sheets are fixedly provided on the lifting seat, and each of the anti-sinking sheets is provided with a plurality of material penetration holes;

[0018] A protective plate is fixedly arranged on each of the anti-sinking sheets.

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

[0020] A plurality of springs are provided between the lifting seat and the carrying cylinder, and two ends of the plurality of springs are fixedly connected to the lifting seat and the carrying cylinder respectively.

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

[0022] The abutting rod and the abutting pin are both provided with inclined surfaces.

[0023] Preferably, it further comprises a reciprocating screw, wherein the reciprocating screw is provided with a sliding groove, and the supporting cylinder located at the bottom is provided with a fixed block, and the fixed block is slidably provided in the sliding groove;

[0024] The supporting cylinder at the bottom is slidably connected to the reactor, and the supporting cylinder at the top is fixedly connected to the reactor;

[0025] The reciprocating screw is in abutment with a lifting seat on the lowermost supporting cylinder.

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

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

[0028] In the above technical solution, the method for purifying trimethylsilane provided by the present invention has the following beneficial effects:

[0029] 1. The chlorine-containing organic impurities in the magnesium chips and crude trimethylsilane are removed, and the trimethylsilane after the reaction is evaporated. Then, light components such as dimethylsilane are removed by distillation to complete the purification of the distilled trimethylsilane. After testing, this method has low cost, high purity of trimethylsilane, and low complexity.

[0030] 2. During the reaction of crude chlorinated trimethylsilane and magnesium chips, the magnesium chips are placed in multiple supporting tubes and the supporting tubes are located at different heights during the reaction to prevent the magnesium chips from settling at the bottom of the reactor, resulting in insufficient reaction and excessive stirring time. At the same time, anti-sinking parts are set to prevent magnesium chips from accumulating in the reactor, reducing the contact area between the magnesium chips and the crude chlorinated trimethylsilane, thereby effectively improving the reaction efficiency.

[0031] It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.

[0032] This application document provides an overview of various implementations or examples of the technology described in this disclosure, and is not a comprehensive disclosure of the full scope or all features of the disclosed technology. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments. Obviously, the drawings described below are only some embodiments described in the present invention. For ordinary technicians in this field, other drawings can also be obtained based on these drawings.

[0034] Figure 1A schematic diagram of the internal structure of a reactor provided in an embodiment of the present invention;

[0035] Figure 2 A schematic diagram of the structure of each bearing tube provided in an embodiment of the present invention;

[0036] Figure 3 The embodiment of the present invention provides Figure 2 A magnified view of point A in the figure;

[0037] Figure 4 The embodiment of the present invention provides Figure 2 Enlarged view of point B in FIG.

[0038] Figure 5 A schematic diagram of the anti-sinking structure provided by 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] Description of reference numerals:

[0041] 1. Reactor; 11. Stirring shaft; 12. Ratchet block; 13. Feed port; 14. Motor; 2. Carrying cylinder; 21. Fixed block; 3. Rotating frame; 31. Spring; 4. Lifting seat; 41. Anti-sinking plate; 42. Protective plate; 43. Feeding 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 DESCRIPTION

[0042] To make the purpose, technical solutions, and advantages of the embodiments of the present disclosure more clear, the technical solutions of the embodiments of the present disclosure will be clearly and completely described below in conjunction with the accompanying drawings of the embodiments of the present disclosure. Obviously, the described embodiments are part of the embodiments of the present disclosure, not all of the embodiments. Based on the described embodiments of the present disclosure, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present disclosure.

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

[0044] S1: Add magnesium chips into reactor 1 under an inert gas environment, control the temperature of reactor 1 to -20~0°C, add crude trimethylsilane containing chlorine into reactor 1, start stirring, and keep the condenser temperature at -30~-20°C;

[0045] S2: Control the pressure of reactor 1 to 300 kPa, the temperature to 30-35 °C, and stir for 6 hours;

[0046] S3: After the stirring is completed, the normal pressure is restored to evaporate the trimethylsilane, which is collected in a crude product receiving tank and finally transferred to the distillation bottom kettle;

[0047] S4: Control the distillation bottom kettle pressure to 200KPa and the temperature to 25~30℃ for distillation, and remove light components at a ratio of 5~8%;

[0048] S5: receiving the fraction at about 25°C and collecting it into a receiving tank to complete the purification of trimethylsilane;

[0049] The reactor 1 also includes a grading component, which is used to grade the magnesium chips in step S1. The grading component includes multiple supporting tubes 2, each of which is slidably connected and abutted. Each supporting tube 2 is provided with an anti-sinking part to prevent the magnesium chips from settling at the bottom of the supporting tube 2.

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

[0051] The amount of magnesium chips 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, and the chloride ion content thereof was analyzed and tested to be 5000 ppm, and the chloride ion content was approximately 717.1 g (20.2 mol);

[0054] 2. Under the protection of inert gas, transfer 0.73 kg of magnesium chips to the reactor for replacement (the total value of other gases and water is less than 1 ppm). Control the temperature of the reactor at -10~0°C. Then transfer 300 kg of crude trimethylsilane (containing chlorine) to the reactor. Start stirring and control the condenser temperature at -30~-20°C.

[0055] 3. Control the reactor pressure at 300 kPa and the temperature at 30 °C, and stir for 6 hours. After the stirring is completed, the pressure is restored to normal pressure and trimethylsilane is evaporated and collected in a crude product receiving tank, and finally transferred to the distillation bottom kettle;

[0056] 4. The distillation bottom kettle is controlled at a pressure of 200KPa and a temperature of 25-30℃ for distillation. The light components are removed at a ratio of 5%, and then 247.8Kg of the fraction at about 25℃ is collected in a product tank, which is the finished trimethylsilane product.

[0057] In this case, the trimethylsilane purification yield was 82.6%. IC, GC, and ICP tests showed that all inorganic elements in the product were less than 1 ppm, including chlorine less than 0.7 ppm, and the purity reached 6N.

[0058] Example 2

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

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

[0061] 3. Control the reactor pressure at 300 kPa and the temperature at 30 °C, and stir for 6 hours. After the stirring is completed, the pressure is restored to normal pressure and trimethylsilane is evaporated and collected in a crude product receiving tank, and finally transferred to the distillation bottom kettle;

[0062] 4. The distillation bottom kettle is controlled at a pressure of 200KPa and a temperature of 25-30℃ for distillation. The light components are removed at a ratio of 8%. Then, 251Kg of the fraction at about 25℃ is collected in a product tank, which is the finished trimethylsilane product.

[0063] In this case, the trimethylsilane purification yield was 81.5%. IC, GC, and ICP tests showed that all inorganic elements in the product were less than 1 ppm, including chlorine less than 0.5 ppm, and the purity reached 6N.

[0064] Example 3

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

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

[0067] 3. Control the reactor pressure at 300 kPa and the temperature at 30 °C, and stir for 6 hours. After the stirring is completed, the pressure is restored to normal pressure and trimethylsilane is evaporated and collected in a crude product receiving tank, and finally transferred to the distillation bottom kettle;

[0068] 4. The distillation bottom kettle is controlled at a pressure of 200KPa and a temperature of 25-30°C for distillation. The light components are removed at a ratio of 6%, and then 256.2Kg of the fraction at about 25°C is collected in a product tank, which is the finished trimethylsilane product.

[0069] In this case, the trimethylsilane purification yield was 82.1%. IC, GC, and ICP tests showed that all inorganic elements in the product were less than 1 ppm, including chlorine less than 0.6 ppm, and the purity reached 6N.

[0070] During the reaction of crude chlorinated trimethylsilane and magnesium chips, the magnesium chips are put into multiple supporting tubes 2 and the supporting tubes 2 are located at different heights during the reaction to prevent the magnesium chips from settling at the bottom of the reactor 1 during the reaction, resulting in insufficient reaction and excessive stirring time. At the same time, anti-sinking parts are set to prevent the magnesium chips from accumulating in the reactor 1, reducing the contact area between the magnesium chips and the crude chlorinated trimethylsilane, thereby effectively improving the reaction efficiency.

[0071] Specifically, the anti-sinking part includes a lifting seat 4, which is fitted with the carrying cylinder 2. A plurality of anti-sinking sheets 41 are fixedly provided on the lifting seat 4, and a plurality of penetration holes 43 are provided on each anti-sinking sheet 41; a protective plate 42 is fixedly provided on each anti-sinking sheet 41. During the reaction process of the crude chlorinated trimethylsilane and the magnesium chips, the motor 14 drives the stirring shaft 11 to rotate the lifting seat 4 synchronously, and the lifting seat 4 and the anti-sinking sheet 41 rotate to prevent the magnesium chips from settling on the lifting seat 4 and to make the magnesium chips pass through the lifting seat 4 after being lifted up. The feeding hole 43 prevents magnesium chips from adhering to the anti-sinking sheet 41, thereby increasing the contact area between the crude chlorinated trimethylsilane and the magnesium chips and improving the reaction rate. A protective plate 42 is provided on the anti-sinking sheet 41 to prevent the magnesium chips lifted by the anti-sinking sheet 41 from escaping from the supporting tube 2 and then settling at the bottom of the reactor 1. During the reaction, multiple supporting tubes 2 are located at different heights in the reactor 1, which can further improve the effect of the reaction between the crude chlorinated trimethylsilane and the magnesium chips and avoid insufficient reaction.

[0072] In an embodiment further provided by the present invention, a rotating frame 3 is rotatably provided on the supporting 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 supporting cylinder 2, and the two ends of the plurality of springs 31 are fixedly connected to the lifting seat 4 and the supporting cylinder 2 respectively. During the reaction process, 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 moved downward, the spring 31 is stretched, and the lifting seat 4 is separated from the supporting cylinder 2. Since the contact surface between the lifting seat 4 and the supporting cylinder 2 is an inclined surface, the by-products or incompletely reacted magnesium chips generated inside the supporting cylinder 2 can be discharged and deposited to the bottom position of the reactor 1.

[0073] Furthermore, a stirring shaft 11 is rotatably provided on the reactor 1, an abutment pin 44 is fixedly provided on the lifting seat 4, an abutment rod 8 is fixedly provided 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, and magnesium chips are put into each supporting cylinder 2, and each supporting cylinder 2 slides down to a different height, and the abutment pin 44 on the lifting seat 4 on each supporting cylinder 2 also moves down to a position relative to each abutment rod 8, and the stirring shaft 11 rotates, and stirring is performed by the stirring blade on the stirring shaft 11, and at the same time the abutment rod 8 rotates and engages with the corresponding abutment pin 4 during the rotation process. 4 abuts, and after the abutment, the lifting seat 4 is rotated by the abutment pin 44, so that the lifting seat 4 and the rotating frame 3 rotate, and the anti-sinking piece 41 prevents magnesium chips from settling at the bottom of the carrying cylinder 2. By providing inclined surfaces on the abutment pin 44 and the abutment rod 8, if the carrying cylinder 2 is in the process of descending, the abutment pin 44 and the abutment rod 8 are at the same angle and collide with each other, the mutual squeezing of the inclined surfaces can restrict the descent of the carrying cylinder 2. When the abutment rod 8 rotates, it abuts against the upper part of the inclined surface on the abutment pin 44, thereby pushing the lifting seat 4 to rotate, thereby improving the rotation stability of the lifting seat 4.

[0074] Furthermore, it also includes a reciprocating screw 5, which is provided with a sliding groove 51, and a fixed block 21 is provided on the bearing cylinder 2 at the bottom, and the fixed block 21 is slidably set in the sliding groove 51; and the bearing cylinder 2 at the bottom is slidably connected to the reactor 1, and the bearing cylinder 2 at the top is fixedly connected to the reactor 1; the reciprocating screw 5 is in abutment with the lifting seat 4 on the bearing cylinder 2 at the bottom. When magnesium chips are put in, each bearing cylinder 2 is at the same height at the top. After the magnesium chips are put into each bearing cylinder 2, the reciprocating screw 5 moves down with the bottom bearing cylinder 2. At this time, under the action of gravity, except for the top bearing cylinder 2, the other bearing cylinders 2 all move down. Because the top bearing cylinder 2 is fixedly connected to the reactor 1, when each bearing cylinder 2 moves down, the bearing cylinder 2 When it contacts the lifting seat 4 of the upper supporting cylinder 2, it is restricted from moving downward by the force of the spring 31, so that each supporting cylinder 2 stops at a different height. After the reaction is completed, the reciprocating screw 5 continues to move downward, pressing the lowest supporting cylinder 2, so that the adjacent lifting seat 4 moves downward. The spring 31 stretches, and after stretching, while continuing to move the lower supporting cylinder 2 downward, each supporting cylinder 2 moves downward with the lifting seat 4 on the adjacent supporting cylinder 2, so that the lifting seat 4 on each supporting cylinder 2 is separated from the corresponding supporting cylinder 2, so that the reaction by-products or incompletely reacted magnesium chips in the supporting cylinder 2 are precipitated from the supporting cylinder 2 and accumulated at the position of the discharge port at the bottom of the reactor 1, so as to facilitate the cleaning of the products inside the reactor 1 after the reaction.

[0075] When the supporting tube 2 rises, the reciprocating screw 5 moves the bottom supporting tube 2 upward, and when it moves to the same height as the adjacent supporting tube 2, it abuts against the adjacent supporting tube 2 and drives it to move upward. In turn, each supporting tube 2 can be moved up to the position of the feed port 13 at the top of the reactor 1 by the upward movement of the reciprocating screw 5. The shape and size of the feed port 13 can be adjusted according to actual application to facilitate the more convenient feeding of magnesium chips into each supporting tube 2.

[0076] In an embodiment further provided by the present invention, a first pulley 6 and a second pulley 7 are rotatably provided 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. The second pulley 7 rotates to drive the first pulley 6 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 ascent and descent of the reciprocating screw 5, thereby completing the ascent and descent of the carrier cylinder 2.

[0077] When each supporting cylinder 2 is moved down to the position of the reaction height, the top end of the reciprocating screw 5 does not drop to contact with 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 down, completing the separation of each supporting cylinder 2 from the corresponding lifting seat 4. When the product inside the supporting cylinder 2 is precipitated, the top end of the reciprocating screw 5 contacts the first pulley 6. After the product inside the supporting cylinder 2 is precipitated, the first pulley 6 continues to rotate. Under the characteristics of the reciprocating screw 5, the reciprocating screw 5 rises and causes each supporting cylinder 2 to rise to the feeding position.

[0078] In the embodiment provided by the present invention, a ratchet block 12 is rotatably provided on the stirring shaft 11, and a ratchet ring 71 is fixedly provided on the second pulley 7. The ratchet block 12 is engaged with the ratchet ring 71, and a torsion spring is provided between the ratchet block 12 and the stirring shaft 11. By providing the ratchet block 12 and the ratchet ring 71, the motor 14 drives the stirring shaft 11 to rotate, and 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 to realize the lifting and lowering of the reciprocating screw 5. After the reciprocating screw 5 is lifted and lowered, the motor 14 drives the stirring shaft 11 to reverse. When the stirring reaction is carried out, 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, so the first pulley 6 and the second pulley 7 will not rotate, so that the reciprocating screw 5 remains stable to maintain the stability of each supporting cylinder 2.

[0079] The above description is merely illustrative of certain exemplary embodiments of the present invention. It goes without saying that those skilled in the art will be able to modify the described embodiments in various ways without departing from the spirit and scope of the present invention. Therefore, the above drawings and description are illustrative in nature and should not be construed as limiting the scope of protection of the claims.

Claims

1. A method for purifying trimethylsilane, characterized in that: The following steps are involved: S1: Add magnesium chips into the reactor (1) under an inert gas environment, control the temperature of the reactor (1) to -10~0°C, add crude trimethylsilane containing chlorine into the reactor (1), start stirring, and keep the condenser temperature at -30~-20°C; S2: Control the reactor pressure to 300 kPa, the temperature to 30-35 °C, and stir for 6 h; S3: After the stirring is completed, the normal pressure is restored to evaporate the trimethylsilane, which is collected in a crude product receiving tank and finally transferred to the distillation bottom kettle; S4: Control the distillation bottom kettle pressure to 200KPa and the temperature to 25~30℃ for distillation, and remove light components at a ratio of 5~8%; S5: receiving the fraction at about 25°C and collecting it into a receiving tank to complete the purification of trimethylsilane; The reactor (1) further comprises a grading assembly for grading the magnesium chips in step S1, the grading assembly comprising a plurality of supporting cylinders (2), each of the supporting cylinders (2) being slidably connected and abuttingly fitted, and each of the supporting cylinders (2) being provided with an anti-sinking member for preventing the magnesium chips from settling at the bottom of the supporting cylinder (2).

2. The method for purifying trimethylsilane according to claim 1, wherein The steps S1 to S5 are all carried out under the protection of an inert gas, 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, wherein In the S1, the amount of magnesium chips is 1.5 to 4 times the chloride ion content.

4. The method for purifying trimethylsilane according to claim 1, wherein The anti-sinking component comprises a lifting seat (4), the lifting seat (4) is fitted with the supporting tube (2), a plurality of anti-sinking plates (41) are fixedly provided on the lifting seat (4), and each of the anti-sinking plates (41) is provided with a plurality of penetration holes (43); A protective plate (42) is fixedly provided on each of the anti-sinking sheets (41).

5. The method for purifying trimethylsilane according to claim 4, wherein: A rotating frame (3) is rotatably provided on the bearing 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 bearing cylinder (2), and two ends of the plurality of 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, wherein: The reactor (1) is rotatably provided with a stirring shaft (11), the lifting seat (4) is fixedly provided with an abutment pin (44), the stirring shaft (11) is fixedly provided with an abutment rod (8), and the abutment rod (8) is adapted to the abutment pin (44); The abutment rod (8) and the abutment pin (44) are both provided with inclined surfaces.

7. The method for purifying trimethylsilane according to claim 4, wherein: It also includes a reciprocating screw (5), the reciprocating screw (5) is provided with a sliding groove (51), and the supporting cylinder (2) located at the bottom is provided with a fixed block (21), and the fixed block (21) is slidably arranged in the sliding groove (51); The supporting cylinder (2) located at the bottom is slidably connected to the reactor (1), and the supporting cylinder (2) located at the top is fixedly connected to the reactor (1); The reciprocating screw (5) is in abutment with the lifting seat (4) on the lowermost supporting cylinder (2).

8. The method for purifying trimethylsilane according to claim 7, wherein: A first pulley (6) and a second pulley (7) are rotatably provided 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.

9. The method for purifying trimethylsilane according to claim 7, wherein: A ratchet block (12) is rotatably provided on the stirring shaft (11), a ratchet ring (71) is fixedly provided on the second pulley (7), the ratchet block (12) and the ratchet ring (71) are engaged with each other, and a torsion spring is provided between the ratchet block (12) and the stirring shaft (11).

Citation Information

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