A purification method and purification processing system for diiodosilane

Abstract

The invention discloses a diiodosilane purification method and a purification processing system, relating to the technical field of diiodosilane. A driving component is provided on a mounting shell, an inner liner is clamped on an output end of the driving component, the driving component is slidably connected to a sliding groove provided on the mounting shell, the inner liner is located in a sliding cavity in the mounting shell, the sliding cavity is communicated with the sliding groove, a limiting component is installed on the mounting shell, a notch is provided on the mounting shell, the limiting component is tilted toward the notch, and the crystals can be quickly taken out by taking out the inner liner, thereby enhancing work efficiency, facilitating the rapid removal of the crystals, and enabling the next crystallization to be carried out quickly. Moreover, by arranging a filter screen and a railing on the inner liner, the residual liquid in the inner liner can be quickly discharged, thereby preventing the residual liquid from affecting the purity of the diiodosilane.

Description

Technical Field

[0001] The present invention relates to the technical field of diiodosilane, in particular to a diiodosilane purification method and a purification processing system. Background Art

[0002] Diiodosilane (DIS) is an advanced silicon-based precursor material primarily used in semiconductor manufacturing and thin film deposition. Its molecular formula is H2I2Si, and it has multiple synthesis routes, including those using silane and hydrogen iodide, diphenylsilane and hydrogen iodide, and phenylsilane and elemental iodine as raw materials.

[0003] After searching the publication number CN221789299U, a reactor for producing diiodosilane was found, comprising a reactor body, wherein a heating chamber and a reaction chamber that are interconnected are provided inside the reactor body, and a raised end is provided at the bottom of the reaction chamber; a cover plate, wherein the cover plate is connected to the upper end of the reactor body; a mixing mechanism, comprising a driving part, a stirring part and a plurality of material conveying barrels; the driving part is arranged above the cover plate, and is used to drive the stirring part arranged in the reaction chamber to mix and stir the materials; the material conveying barrel is arranged in the heating chamber, and is used to return the materials to the reaction chamber, and a plurality of heating parts are provided in the heating chamber. The invention solves the technical problem that the stirring efficiency of the reactor in the prior art is low when mixing the raw materials for producing diiodosilane, which causes some materials to be easily electrostatically formed at the bottom of the reactor, thereby affecting the quality of subsequent products;

[0004] However, the crude diiodosilane needs to be purified, so it needs to be crystallized and purified. However, the crystallized diiodosilane will stick to the reaction chamber, making it difficult to remove the crystals. At this time, the diiodosilane is at a low temperature and cannot be easily touched, further increasing the difficulty of removing the crystals. Summary of the Invention

[0005] The object of the present invention is to provide a purification method and purification processing system for diiodosilane to solve the deficiencies in the above-mentioned prior art.

[0006] In order to achieve the above object, the present invention provides the following technical solutions:

[0007] Follow these steps:

[0008] S1. Collect crude diiodosilane liquid;

[0009] S2, distilling the crude diiodosilane liquid, the boiling point of diiodosilane is about 210°C;

[0010] S3, collecting the condensed fraction to remove low-boiling-point impurities;

[0011] S4. The distilled fraction is subjected to freeze crystallization. The freezing point of diiodosilane is about -57°C.

[0012] S5, filtering to obtain crystals to remove high-boiling-point impurities;

[0013] S6. Adding a reagent that reacts with the impurities without affecting the diiodosilane;

[0014] S7. Distill and filter to remove residual impurities.

[0015] Furthermore, the invention comprises a mounting shell, wherein a drive assembly is provided on the mounting shell, an inner liner is clamped on the output end of the drive assembly, the drive assembly is slidably connected to a sliding groove provided on the mounting shell, the inner liner is located in a sliding cavity in the mounting shell, the sliding cavity is connected to the sliding groove, and the sliding cavity can collect the fraction in S and can withstand freezing to crystallize the fraction;

[0016] A limiting component is installed on the installation shell. A notch is provided on the installation shell, and the limiting component is tilted toward the notch.

[0017] Furthermore, the drive assembly includes an electric telescopic rod arranged on the mounting shell, the output end of the electric telescopic rod is rotatably connected to a disc member, the disc member is penetrated and fixedly connected by four clamping columns, and two first spring telescopic members are respectively provided on the four clamping columns, and a bevel block is respectively provided on the output end of several first spring telescopic members.

[0018] Furthermore, two second spring telescopic parts are fixed on each of the four clamping columns, and a connecting part is provided on each output end of the plurality of second spring telescopic parts. The plurality of connecting parts are fixedly connected to one end of the plurality of first wires respectively and one by one, and the other ends of the plurality of first wires are connected to the plurality of inclined blocks respectively and one by one.

[0019] Furthermore, the driving assembly further includes a limit block fixedly arranged on the disc member, and the limit block is slidably connected in the sliding groove.

[0020] Furthermore, the bottom of the inner liner is set as a filter, the side of the inner liner is set as a number of railings, and four clips are provided on the inner liner. Four clips are respectively provided with four clip grooves, and the four clip grooves respectively correspond to the positions of the four clip columns.

[0021] Furthermore, the limit assembly includes two limit units, the limit units include two third spring telescopic parts fixedly arranged in the mounting shell, a limit member is provided at the output end of the two third spring telescopic parts, the limit member passes through the sliding cavity, an inclined surface is provided on the limit member, the inclined direction of the inclined surface is toward the notch, and the limit member is fixedly connected to one end of a second wire.

[0022] Furthermore, one end of the two second wires away from the limiting member is fixedly connected to a pressing block, the pressing block is fixedly arranged at an output end of a fourth spring expansion member, and the fourth spring expansion member is fixedly arranged on the mounting shell.

[0023] Furthermore, a slope is provided on the mounting shell, the slope is connected to the two inclined surfaces, the slope is located at the sliding groove, and a storage box is provided on the mounting shell, and the storage box corresponds to the position of the sliding groove.

[0024] Furthermore, the bottom surfaces of the two limiting members are each provided with an inclined surface.

[0025] In the above technical solution, the present invention provides a method for purifying diiodosilane and a purification processing system, which is as follows: an inner liner is placed under a disc so that the four clamping grooves correspond to the positions of the four clamping posts, and then the inner liner is moved upward so that the four clamping parts correspond to the four clamping posts one by one, and the diiodosilane solution to be purified is injected into the sliding cavity. Then, the electric telescopic rod is started to drive the disc to move downward, and sealing rubber rings are set on the four sides of the disc so that the diiodosilane solution to be purified is sealed. The diiodosilane solution to be purified is then crystallized. The crystallized diiodosilane will adhere to the inside of the sliding cavity. Before moving downward, the pressing block is pressed to contract the fourth spring telescopic member, driving the two second wires to be pulled, so that the two limit members are pulled, so that the existence of the limit members will not affect the downward movement of the inner tank member. Then, the electric telescopic rod is started to drive the disc member to move upward. The setting of the sliding groove makes the limit block rotate when moving upward, driving the inner tank member to rotate, so that the diiodosilane crystals no longer adhere to the inner tank of the sliding cavity. , so that the inner tank can be quickly taken out, so that the crystal can be quickly taken out, which enhances work efficiency, facilitates the rapid removal of the crystal, and enables the next crystallization to be carried out quickly. Moreover, through the setting of the filter screen and the railing on the inner tank, the residual liquid in the inner tank will be quickly discharged, preventing the residual liquid from affecting the purity of diiodosilane. After that, the disc drives the inner tank to move upward, so that several connecting parts are in contact with the top of the sliding cavity, so that the four clamping columns are no longer clamped with the four clamping parts. At this time, the inner tank falls to the two On the limiting part, the inner liner part slides through the setting of the inclined surfaces on the two limiting parts, and the inner liner part slides into the storage box for collection through the setting of the slope and the groove, and the solution other than the residual crystals in the inner liner part is thrown out by the vibration force of the fall when the inner liner part falls, further ensuring the purity of diiodosilane. After that, the electric telescopic rod drives the disc part to move downward, so that several second spring telescopic parts are released, so that several first spring telescopic parts are released, and drive several inclined blocks to reset, so as to facilitate the clamping with the next inner liner part. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] 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.

[0027] Figure 1 One of the structural diagrams provided in an embodiment of the present invention;

[0028] Figure 2 The second structural diagram provided for an embodiment of the present invention;

[0029] Figure 3 One of the internal structure diagrams provided in an embodiment of the present invention;

[0030] Figure 4 The second internal structure diagram provided by the embodiment of the present invention;

[0031] Figure 5 One of the partial structural diagrams provided in an embodiment of the present invention;

[0032] Figure 6 This is the second partial structural diagram provided for an embodiment of the present invention.

[0033] Description of reference numerals:

[0034] 1. Mounting shell; 11. Sliding groove; 12. Sliding cavity; 13. Notch; 14. Slope; 15. Storage box; 2. Drive assembly; 21. Electric telescopic rod; 22. Disc; 23. Snap-on column; 24. First spring telescopic member; 25. Oblique block; 26. Second spring telescopic member; 27. Connecting member; 28. First conductor; 29. ​​Limiting block; 3. Inner liner; 31. Filter; 32. Railing; 33. Snap-on member; 4. Limiting assembly; 41. Limiting unit; 411. Third spring telescopic member; 412. Limiting member; 413. Second conductor; 42. Pressing block; 43. Fourth spring telescopic member. DETAILED DESCRIPTION

[0035] In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings.

[0036] See also Figure 1-6 The embodiment of the present invention provides a method and system for purifying diiodosilane, which comprises the following steps:

[0037] S1. Collect crude diiodosilane liquid;

[0038] S2, distilling the crude diiodosilane liquid, the boiling point of diiodosilane is about 210°C;

[0039] S3, collecting the condensed fraction to remove low-boiling-point impurities;

[0040] S4. The distilled fraction is subjected to freeze crystallization. The freezing point of diiodosilane is about -57°C.

[0041] S5, filtering to obtain crystals to remove high-boiling-point impurities;

[0042] S6. Adding a reagent that reacts with the impurities without affecting the diiodosilane;

[0043] S7. Distill and filter to remove residual impurities.

[0044] Preferably, it includes a mounting shell 1, on which a drive assembly 2 is provided, an inner liner 3 is clamped on the output end of the drive assembly 2, the drive assembly 2 is slidably connected to a sliding groove 11 provided on the mounting shell 1, the inner liner 3 is located in a sliding cavity 12 in the mounting shell 1, the sliding cavity 12 is connected to the sliding groove 11, and the sliding cavity 12 can collect the fraction in S4 and can withstand freezing to crystallize the fraction;

[0045] The mounting shell 1 is provided with a limit assembly 4 . A notch 13 is provided on the mounting shell 1 , and the limit assembly is tilted toward the notch.

[0046] Preferably, the drive assembly 2 includes an electric telescopic rod 21 arranged on the mounting shell 1, and the output end of the electric telescopic rod 21 is rotatably connected to a disc member 22. The disc member 22 is penetrated and fixedly connected by four clamping columns 23. Two first spring telescopic members 24 are respectively provided on the four clamping columns 23, and a plurality of first spring telescopic members 24 are respectively provided with an inclined block 25 on the output end. Through the cooperation of the first spring telescopic member 24 and the inclined block 25, the drive assembly 2 can be clamped and released with the inner tank member 3, which facilitates the limitation and collection of the inner tank member 3.

[0047] Preferably, two second spring telescopic members 26 are fixed on each of the four clamping columns 23, and a connecting member 27 is provided on each output end of the second spring telescopic members 26. The connecting members 27 are fixedly connected to one end of the first wires 28 respectively and one by one, and the other ends of the first wires 28 are connected to the inclined blocks 25 respectively and one by one. When the connecting members 27 move up to contact the top of the sliding cavity 12, the second spring telescopic members 26 are contracted, driving the inclined blocks 25 to be pulled, so that the drive assembly 2 can be released from the inner tank part 3, so that the inner tank part 3 can fall off, and the solution other than the residual crystals in the inner tank part 3 is thrown out by the vibration force of the fall, further ensuring the purity of diiodosilane.

[0048] Preferably, the drive assembly 2 also includes a limit block 29 fixedly provided on the disc member 22, and the limit block 29 is slidably connected in the sliding groove 11. Through the cooperation of the limit block 29 and the limit groove, the inner tank member 3 can be rotated first when moving upward, so that the crystals are no longer adhered to the sliding cavity 12, so that the crystals can be quickly taken out.

[0049] Preferably, the bottom of the inner liner 3 is set as a filter 31, the side of the inner liner 3 is set as a number of railings 32, and four clips 33 are provided on the inner liner 3. Four clip grooves are respectively opened on the four clips 33, and the four clip grooves respectively correspond to the positions of the four clip columns 23. Through the setting of the four clip grooves, the drive assembly 2 can be clipped with the inner liner 3.

[0050] Preferably, the limiting assembly 4 includes two limiting units 41, and the limiting unit 41 includes two third spring telescopic parts 411 fixedly arranged in the mounting shell 1. A limiting part 412 is provided at the output end of the two third spring telescopic parts 411, and the limiting part 412 extends into the sliding cavity 12. An inclined surface is provided on the limiting part 412, and the inclined direction of the inclined surface is toward the slot 13. The limiting part 412 is fixedly connected to one end of a second wire 413. Through the cooperation between the third spring telescopic part 411 and the limiting part 412, the upward movement of the inner liner part 3 will not be blocked, but the falling of the inner liner part 3 will be caused by the setting of the inclined surface, so that the inner liner part 3 can slide to the outside of the mounting shell 1 so that the inner liner part 3 can be collected.

[0051] Preferably, one end of the two second wires 413 away from the limiting member 412 is fixedly connected to a pressing block 42, and the pressing block 42 is fixedly set at the output end of a fourth spring telescopic member 43, and the fourth spring telescopic member 43 is fixedly set on the mounting shell 1. Through the cooperation between the pressing block 42 and the second wire 413, pressing the pressing block 42 can make the limiting member 412 withdraw from the sliding cavity 12, so that the setting of the limiting member 412 will not affect the next placement of the inner tank member 3.

[0052] Preferably, a slope 14 is provided on the mounting shell 1, and the slope 14 is connected to the two inclined surfaces. The slope 14 is located at the sliding groove 11. A storage box 15 is provided on the mounting shell 1, and the storage box 15 corresponds to the position of the sliding groove 11. The setting of the slope 14 can ensure that the inner liner 3 enters the storage box 15 to ensure that the inner liner 3 can be collected.

[0053] Preferably, the bottom surface of each of the two limiting members 412 is provided with an inclined surface, and the inclined surface can push the two limiting members 412 apart when the inner liner 3 moves upward, so that the two limiting members 412 will not affect the upward movement of the inner liner 3.

[0054] Working principle: By placing the inner container 3 under the disc 22, the four engaging grooves correspond to the positions of the four engaging posts 23 respectively. Then, the inner container 3 is moved upward, so that the inclined blocks 25 contact the four engaging grooves respectively, causing the first spring expansion members 24 to contract, driving the inclined blocks 25 to be respectively retracted into the four engaging posts 23. When the inner container 3 moves upward until it no longer contacts the inclined blocks 25, the four first spring expansion members 24 are released, driving the four inclined blocks 25 to be released, so that the four engaging members 33 are respectively engaged with the four engaging posts 23 in a one-to-one correspondence.

[0055] The diiodosilane solution to be purified is injected into the sliding cavity 12, and then the electric telescopic rod 21 is started to drive the disc 22 to move downward, so that the limit block 29 moves downward. The setting of the sliding groove 11 limits the movement of the limit block 29, so that the disc 22 rotates after falling to a certain position, driving the plurality of clamping columns 23 to rotate, so that the inner liner 3 rotates until the inner liner 3 falls to the bottom side of the sliding cavity 12. At the same time, sealing rubber rings are provided on the four sides of the disc 22 to seal the diiodosilane solution to be purified. Then, the diiodosilane solution to be purified is crystallized, and the crystallized diiodosilane will adhere to the interior of the sliding cavity 12.

[0056] Before moving downward, the pressing block 42 is pressed to contract the fourth spring expansion member 43, which drives the two second wires 413 to be pulled, thereby pulling the two limit members 412, so that the presence of the limit members 412 does not affect the downward movement of the inner container 3;

[0057] The electric telescopic rod 21 is started to drive the disc part 22 to move upward, so that the limit block 29 moves upward. The setting of the sliding groove 11 makes the limit block 29 rotate when moving upward, driving the disc part 22 to rotate, so that the four clamping posts 23 rotate, and driving the inner tank part 3 to rotate, so that the diiodosilane crystals no longer adhere to the inner tank of the sliding cavity 12, so that the crystals are located inside the inner tank part 3. Then the disc part 22 drives the inner tank part 3 to move upward, so that the disc part 22 contacts the inclined surfaces of the two limit parts 412, driving the two third spring telescopic parts 411 to contract, so that the two limit parts 412 contract and exit the sliding cavity 12. When the disc part 22 moves up to the point where the inner tank part 3 no longer contacts the two limit parts 412, the two third spring telescopic parts 411 are released, driving the two limit parts 412 to reset. Then the disc part 22 moves up, driving the four clamping posts 23 to move upward, so that several The second spring telescopic parts 26 move upward, driving several connecting parts 27 to move upward, so that several connecting parts 27 contact the top of the sliding cavity 12, driving several second spring telescopic parts 26 to contract, so that several first wires 28 are pulled, driving several inclined blocks 25 to be pulled, so that several first spring telescopic parts 24 contract, so that the four clamping columns 23 are no longer clamped with the four clamping parts 33. At this time, the inner liner part 3 falls onto the two limit parts 412, and the inner liner part 3 slides through the setting of the inclined surfaces on the two limit parts 412, and the inner liner part 3 slides into the storage box 15 for collection through the setting of the slope 14 and the notch 13. After that, the electric telescopic rod 21 drives the disc part 22 to move downward, so that several second spring telescopic parts 26 are released, so that several first spring telescopic parts 24 are released, and driving several inclined blocks 25 to reset, so as to facilitate clamping with the next inner liner part 3. 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 diiodosilane purification processing system, for implementing a diiodosilane purification method, the diiodosilane purification method comprising the following steps: S1, collecting crude diiodosilane liquid; S2, distilling the crude diiodosilane liquid; S3, collecting the condensed fraction to remove low-boiling-point impurities; S4, freezing and crystallizing the distilled fraction; S5, filtering the obtained crystals to remove high-boiling-point impurities; S6, adding a reagent that can react with the impurities without affecting the diiodosilane; S7, distilling and filtering to remove residual impurities; It is characterized by: The invention comprises a mounting shell (1), a driving assembly (2) is provided on the mounting shell (1), an inner liner (3) is clamped on the output end of the driving assembly (2), the driving assembly (2) is slidably connected to a sliding groove (11) provided on the mounting shell (1), the inner liner (3) is located in a sliding cavity (12) in the mounting shell (1), the sliding cavity (12) is communicated with the sliding groove (11), and the sliding cavity (12) can collect the fraction in S4 and can withstand freezing to crystallize the fraction; A limit assembly (4) is installed on the installation shell (1), a notch (13) is provided on the installation shell (1), and the limit assembly (4) is tilted toward the notch; The driving assembly (2) comprises an electric telescopic rod (21) arranged on the mounting shell (1); the output end of the electric telescopic rod (21) is rotatably connected to a disc member (22); the disc member (22) is penetrated and fixedly connected by four clamping columns (23); two first spring telescopic members (24) are respectively arranged on the four clamping columns (23); and a plurality of the first spring telescopic members (24) are respectively provided with an inclined block (25); Two second spring expansion members (26) are fixed on each of the four clamping columns (23); a connecting member (27) is provided on each output end of the plurality of second spring expansion members (26); the plurality of connecting members (27) are fixedly connected to one end of the plurality of first wires (28) in a one-to-one correspondence; and the other ends of the plurality of first wires (28) are connected to the plurality of inclined blocks (25) in a one-to-one correspondence.

2. A diiodosilane purification processing system according to claim 1, characterized in that, The driving assembly (2) further comprises a limit block (29) fixedly arranged on the disc member (22), and the limit block (29) is slidably connected in the sliding groove (11).

3. A diiodosilane purification processing system according to claim 2, characterized in that, The bottom of the inner container (3) is provided with a filter (31), the side of the inner container (3) is provided with a plurality of railings (32), and the inner container (3) is provided with four clamping parts (33), and the four clamping parts (33) are respectively provided with four clamping grooves, and the four clamping grooves respectively correspond to the positions of the four clamping columns (23).

4. A diiodosilane purification processing system according to claim 3, characterized in that, The limiting assembly (4) includes two limiting units (41), the limiting units (41) including two third spring expansion members (411) fixedly arranged in the mounting shell (1), a limiting member (412) being provided at the output end of the two third spring expansion members (411), the limiting member (412) penetrating into the sliding cavity (12), an inclined surface being provided on the limiting member (412), the inclined surface being inclined toward the notch (13), and the limiting member (412) being fixedly connected to one end of a second wire (413).

5. A diiodosilane purification processing system according to claim 4, characterized in that, One end of the two second conductive wires (413) away from the limiting member (412) is fixedly connected to a pressing block (42), the pressing block (42) is fixedly arranged at the output end of a fourth spring expansion member (43), and the fourth spring expansion member (43) is fixedly arranged on the mounting shell (1).

6. A diiodosilane purification processing system according to claim 5, characterized in that: The mounting shell (1) is provided with a slope (14), the slope (14) is connected to the two inclined surfaces, the slope (14) is located at the sliding groove (11), and the mounting shell (1) is provided with a storage box (15), the storage box (15) corresponds to the position of the sliding groove (11).

7. A diiodosilane purification processing system according to claim 6, characterized in that: The bottom surfaces of the two limiting members (412) are each provided with an inclined surface.

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