CN116789140A - Diiodosilane and preparation method thereof - Google Patents
Diiodosilane and preparation method thereof Download PDFInfo
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- CN116789140A CN116789140A CN202310789246.0A CN202310789246A CN116789140A CN 116789140 A CN116789140 A CN 116789140A CN 202310789246 A CN202310789246 A CN 202310789246A CN 116789140 A CN116789140 A CN 116789140A
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- Prior art keywords
- mixing
- diiodosilane
- compounding
- assembly
- pipe
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- AIHCVGFMFDEUMO-UHFFFAOYSA-N diiodosilane Chemical compound I[SiH2]I AIHCVGFMFDEUMO-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 160
- 238000011049 filling Methods 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000004821 distillation Methods 0.000 claims abstract description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 28
- 239000011630 iodine Substances 0.000 claims description 28
- 229910052740 iodine Inorganic materials 0.000 claims description 28
- PARWUHTVGZSQPD-UHFFFAOYSA-N phenylsilane Chemical compound [SiH3]C1=CC=CC=C1 PARWUHTVGZSQPD-UHFFFAOYSA-N 0.000 claims description 28
- 238000013329 compounding Methods 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 19
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 15
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 15
- 241001330002 Bambuseae Species 0.000 claims description 15
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 15
- 239000011425 bamboo Substances 0.000 claims description 15
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 10
- 238000002955 isolation Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000011541 reaction mixture Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000004891 communication Methods 0.000 claims description 4
- 239000012295 chemical reaction liquid Substances 0.000 claims description 3
- 238000000429 assembly Methods 0.000 claims description 2
- 230000000712 assembly Effects 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000005057 refrigeration Methods 0.000 claims description 2
- 230000006978 adaptation Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 24
- 238000004378 air conditioning Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Chemical compound [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 1
- VDCSGNNYCFPWFK-UHFFFAOYSA-N diphenylsilane Chemical compound C=1C=CC=CC=1[SiH2]C1=CC=CC=C1 VDCSGNNYCFPWFK-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 229910000043 hydrogen iodide Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Abstract
The invention discloses a preparation method of diiodosilane, which specifically comprises the following steps: step one, filling; step two, premix; step three, precooling; step four, mixing reaction; step five, micro-reaction; step six, reduced pressure distillation; the invention relates to the technical field of diiodosilane preparation. According to the preparation method of diiodosilane, the driving assembly, the switching assembly, the mixing kettle, the first mixing barrel and the second mixing barrel are matched, raw materials are preliminarily mixed, the precooling of the raw materials in the first mixing barrel and the second mixing barrel is guaranteed under the arrangement of a cold air inlet pipe, the arrangement of the flow guide assembly and the feeding assembly is matched, the raw materials in the first mixing barrel and the second mixing barrel can be accurately injected into the mixing basin, the stirring of the raw materials in the mixing basin is realized by the driving assembly, the micro-channel reactor is not required to be subjected to multiple temperature regulation, the use is more convenient, and the preparation efficiency of diiodosilane is effectively improved.
Description
Technical Field
The invention relates to the technical field of diiodosilane preparation, in particular to a preparation method of diiodosilane.
Background
At present, the diiodosilane synthesis method mainly comprises the following steps: 1. synthesizing diiodosilane by using a method of dichlorosilane and lithium iodide; 2. reacting hydrogen iodide with diphenyl silane; 3. iodine and phenylsilane react, chloroform is used as a solvent, ethyl acetate is used as a catalyst, the iodine and the chloroform are firstly added into a reaction bottle, the phenylsilane and the ethyl acetate are mixed and added dropwise at low temperature, and then the temperature is gradually raised in stages.
The preparation process and apparatus of diiodosilane as claimed in 202210638045.6 includes pre-cooling iodine solution and phenylsilane solution at-40-0 deg.c, mixing reaction at-40-10 deg.c in a micro channel reactor, and subsequent reaction at 20-30 deg.c to synthesize diiodosilane.
Based on the above data, it can be seen that in the process of preparing diiodosilane, the micro-channel reactor needs to be set with different temperatures, the use is more troublesome, the raw materials for preparing diiodosilane need to be stirred and mixed for multiple times, in order to ensure the accurate addition of the raw materials, the high-purity preparation of diiodosilane is ensured, the different raw materials are often required to be stirred independently, and the preparation efficiency of diiodosilane is influenced while the operation is complicated.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a preparation method of diiodosilane, which solves the problems that in the process of diiodosilane preparation, different temperatures are required to be set for a microchannel reactor, the use is troublesome, in order to ensure the high-purity preparation of diiodosilane, different raw materials required in diiodosilane preparation are required to be independently stirred, and the preparation efficiency of diiodosilane is influenced while the operation is cumbersome.
(II) technical scheme
In order to achieve the above purpose, the invention is realized by the following technical scheme: the preparation method of diiodosilane specifically comprises the following steps:
step one, filling: adding iodine and chloroform in a volume ratio of 1:3 into a first mixing cylinder through a feeding pipe, plugging the feeding pipe, adding phenylsilane and ethyl acetate in a mass ratio of 20:1 into a second mixing cylinder through another feeding pipe, and plugging the feeding pipe to finish filling;
step two, premix: step one, in the process of filling, starting a driving assembly, driving the first mixing cylinder and the second mixing cylinder to rotate by the driving assembly through a switching assembly, and obtaining iodine solution in the first mixing cylinder and phenylsilane solution in the second mixing cylinder after filling is completed for a set time;
step three, precooling: the external refrigerating unit guides cold air into the mixing kettle through the cold air inlet pipe to refrigerate, and refrigerates the first mixing cylinder and the second mixing cylinder to realize precooling of iodine solution and phenylsilane solution;
step four, mixing reaction: cold air in the mixing kettle is led into a mixing box for refrigeration, a flow guide assembly is opened, an iodine solution in a first mixing cylinder and a phenylsilane solution in a second mixing cylinder are led into a feeding assembly, the feeding assembly adds the iodine solution and the phenylsilane solution into a mixing basin, and after a driving assembly is started in the second step, the iodine solution and the phenylsilane solution in the mixing basin are stirred to obtain a mixed reaction solution;
step five, micro-reaction: after the stirring in the fourth step is completed, pumping the mixed reaction liquid into a microchannel reactor, and continuing to react in a microchannel at room temperature for a set time to obtain a reaction mixture;
step six, reduced pressure distillation: and (3) rectifying the reaction mixture in the step five under reduced pressure, and collecting a product with the fraction temperature of 35-40 ℃ under 20+/-3 mmHg to obtain the high-purity diiodosilane.
In order to facilitate stable assembly of the first mixing barrel and the second mixing barrel, the invention is further provided with: the top of the mixing kettle is sleeved with a blocking cover, the bottom of the inner cavity of the mixing kettle is fixedly connected with an isolation cylinder, isolation plates are fixedly arranged between the isolation cylinder and the inner wall of the mixing kettle, four isolation plates are arranged and uniformly distributed on the periphery of the isolation cylinder at intervals, the top of the isolation cylinder is fixedly connected with a carrier plate, and the bottom of the carrier plate is fixedly connected with the top of the isolation plate;
the first mixing cylinder and the second mixing cylinder are both provided with two, and the top of the carrier plate is provided with assembly holes matched with the two first mixing cylinders and the two second mixing cylinders.
The invention is further provided with: the driving assembly comprises a driving motor, the driving motor is fixedly mounted at the top of the plugging cover, the output end of the driving motor penetrates through the plugging cover and is fixedly provided with a rotating shaft, the bottom end of the rotating shaft sequentially penetrates through the carrier plate, the isolation cylinder and the mixing kettle, stirring frames are fixedly mounted at the bottom of the plugging cover, the number of the stirring frames is four, and the four stirring frames are respectively matched with the two first mixing cylinders and the two second mixing cylinders.
In order to achieve thorough mixing of the raw materials in the first mixing cylinder and the second mixing cylinder, the invention is further arranged to: the switching subassembly includes four tooth rings and gear, the gear cover is established and fixed mounting is in the periphery of pivot, a plurality of spout has been seted up to the inside of tooth ring, the periphery of first compounding section of thick bamboo and second compounding section of thick bamboo and be located the top fixed mounting of support plate has a plurality of assembly strip, assembly strip and spout matched with use.
In order to ensure that the mixing is always in a low temperature environment, the invention is further arranged to: the bottom fixed mounting of compounding cauldron has the function shell, the bottom of function shell and the top fixed connection of mixing box, the air conditioning advances the pipe intercommunication and fixes in the periphery of compounding cauldron, and the air conditioning advances the pipe setting in the below of carrier plate, the air conditioning advances to be provided with a solenoid electric valve on the pipe, the intercommunicating pore has been seted up on the surface of division board, through the cold air pipe intercommunication between the bottom of compounding cauldron and the mixing box, and the cold air pipe sets up the inside at the function shell.
The invention is further provided with: the two diversion assemblies comprise four diversion pipes which are respectively communicated and fixed at the bottoms of the first mixing cylinder and the second mixing cylinder, four step sleeves are communicated at the bottom of the mixing kettle, and the bottom ends of the diversion pipes penetrate through the mixing kettle and are matched with the step sleeves for use;
the periphery of the step sleeve is sequentially provided with a flowmeter and a second electromagnetic control valve from top to bottom.
In order to realize the interval addition of the raw materials, the invention is further provided with: the feeding assembly comprises a plugging ring and a feeding disc, the bottom of the plugging ring is in sliding contact with the top of the feeding disc, the bottom of the stepped sleeve penetrates through the mixing box and is fixedly mounted at the top of the plugging ring, a first diversion hole communicated with the stepped sleeve is formed in the bottom of the plugging ring, a second diversion hole matched with the first diversion hole is formed in the bottom of the feeding disc, and the second diversion hole is deviated from the stepped sleeve.
The invention is further provided with: the utility model discloses a mixing box, including the bottom, the bottom of mixing box inner chamber, the bottom of pivot is passed through the functional shell and is passed through the mixing box setting, the bottom of mixing box inner chamber is passed through connecting rod fixed mounting in the bottom of mixing box inner chamber, the charging tray sets up and fixed mounting in the periphery of pivot.
In order to ensure effective mixing of the raw materials in the mixing basin, the invention is further provided with: the periphery of pivot and the inside fixed mounting that is located the compounding basin have a plurality of stirring rib pole, the bottom intercommunication of compounding basin has the drain pipe, the one end of drain pipe runs through the mixing box and extends to the periphery of mixing box, and the surface of drain pipe is provided with the third electromagnetic control valve.
The invention is further provided with: the utility model discloses a sealing cover, including the filling tube, the filling tube is provided with four, and four filling tube all runs through the top that sets up at the shutoff lid, four the bottom of filling tube runs through respectively run through to two first compounding section of thick bamboo and second compounding section of thick bamboo in, the top threaded connection of filling tube has the block.
(III) beneficial effects
The invention provides a preparation method of diiodosilane. The beneficial effects are as follows:
(1) According to the invention, raw materials required by diiodosilane preparation are respectively added into the first mixing cylinder and the second mixing cylinder, the driving assembly, the switching assembly and the mixing kettle are matched, the preliminary mixing of the raw materials is realized, the pre-cooling of the raw materials in the first mixing cylinder and the second mixing cylinder is ensured under the arrangement of the cold air inlet pipe, the arrangement of the flow guide assembly and the feeding assembly is matched, the raw materials in the first mixing cylinder and the second mixing cylinder can be accurately injected into the mixing basin, the stirring of the raw materials in the mixing basin is realized by the driving assembly, the effective reaction of the raw materials in a low-temperature environment is ensured, the multi-time temperature adjustment of the micro-channel reactor is not required, the use is more convenient, and the preparation efficiency of diiodosilane is effectively improved.
(2) According to the invention, through the arrangement of the driving motor, the rotating shaft, the gears, the four tooth rings, the first mixing cylinder and the second mixing cylinder, the four tooth rings can be driven to rotate when the driving motor runs, the first mixing cylinder and the second mixing cylinder can be ensured to stably rotate under the cooperation of the sliding chute and the assembling strip, and the arrangement of the stirring frame is used for continuously stirring the raw materials in the first mixing cylinder and the second mixing cylinder and ensuring the uniform mixing of the fillers in the first mixing cylinder and the second mixing cylinder.
(3) According to the invention, through the cooperation of the rotating shaft and the rib rod, when the driving motor operates, the stirring of raw materials in the mixing basin can be realized, the rotating shaft is utilized to drive the feeding disc to rotate while the mixing uniformity of the mixing basin is ensured, the first diversion hole is communicated with the second diversion hole, the raw materials in the first diversion hole can be ensured to flow into the mixing basin through the second diversion hole, the interval addition of the raw materials is realized, and convenience is provided for the full mixing reaction of the raw materials.
(4) According to the invention, through the arrangement of the plugging cover, convenience is provided for taking out the tooth ring, and meanwhile, the first mixing barrel and the second mixing barrel can be conveniently taken out, so that convenience is provided for cleaning the device, and the device is more convenient to use.
Drawings
FIG. 1 is a schematic flow chart of the method of the present invention;
FIG. 2 is a schematic view of the external structure of the mixing kettle, the functional shell and the mixing box of the invention;
FIG. 3 is a schematic diagram of the internal structure of the mixing kettle, the functional shell and the mixing box;
FIG. 4 is a top view of the internal structure of the mixing kettle of the invention;
FIG. 5 is a bottom view of the internal structure of the mixing kettle of the present invention;
FIG. 6 is a schematic structural view of a second mixing barrel and tooth ring of the present invention;
FIG. 7 is a schematic structural view of a second mixing barrel according to the present invention;
FIG. 8 is a schematic view of the structure of the charging assembly of the present invention;
in the figure, 1, a mixing kettle; 2. a blocking cover; 3. an isolation cylinder; 4. a partition plate; 5. a carrier plate; 6. a first mixing cylinder; 7. a second mixing cylinder; 8. a fitting hole; 9. a drive assembly; 10. a driving motor; 11. a rotating shaft; 12. a stirring rack; 13. a switching component; 14. a tooth ring; 15. a gear; 16. a chute; 17. assembling the strip; 18. a functional shell; 19. a mixing box; 20. a cold air inlet pipe; 21. a communication hole; 22. a first solenoid-operated valve; 23. a cold air pipe; 24. a flow guiding pipe; 25. a step sleeve; 26. a flow meter; 27. a second solenoid-operated valve; 28. a charging assembly; 29. a plugging ring; 30. a charging tray; 31. a first deflector aperture; 32. a second deflector aperture; 33. a mixing basin; 34. stirring rib bars; 35. a liquid outlet pipe; 36. a third solenoid-operated valve; 37. a feeding tube; 38. capping; 39. and a flow guiding assembly.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
Referring to fig. 1-8, the following two technical schemes are provided in the embodiments of the present invention:
embodiment 1,
The preparation method of diiodosilane specifically comprises the following steps:
step one, filling: opening the cap 38, adding iodine and chloroform in a volume ratio of 1:3 into the first mixing cylinder 6 through a feeding pipe 37, screwing the cap 38, plugging the feeding pipe 37, taking another feeding pipe 37, opening the cap 38, adding phenylsilane and ethyl acetate in a mass ratio of 20:1 into the second mixing cylinder 7, screwing the cap 38, and plugging the feeding pipe 37 to finish filling;
step two, premix: step one, in the process of filling, starting a driving motor 10, wherein the driving motor 10 is electrically connected with an external power supply, and is controlled by a control switch, the driving motor 10 drives a rotating shaft 11 to rotate, the rotating shaft 11 drives a gear 15 to rotate, the gear 15 drives a tooth ring 14 to rotate, the tooth ring 14 drives an assembly bar 17 to enable a first mixing cylinder 6 and a second mixing cylinder 7 to rotate, and the arrangement of a stirring frame 12 is matched, after the filling setting time is completed, iodine solution is obtained in the first mixing cylinder 6, and phenylsilane solution is obtained in the second mixing cylinder 7;
step three, precooling: the external refrigerating unit is communicated with the cold air inlet pipe 20, the first electromagnetic control valve 22 is opened, the cold air is led into the mixing kettle 1 from the cold air inlet pipe 20 by the external refrigerating unit for refrigerating, and flows into the space below the carrier plate 5 in the mixing kettle 1 through the communication hole 21 to refrigerate the first mixing cylinder 6 and the second mixing cylinder 7, so that precooling of iodine solution and phenylsilane solution is realized;
step four, mixing reaction: the cold air in the mixing kettle 1 is led into the mixing box 19 through the cold air pipe 23 to refrigerate the mixing basin 33, when iodine solution and phenylsilane solution are required to be added into the mixing basin 33, the second electromagnetic control valve 27 on the stepped sleeve 25 corresponding to the first mixing cylinder 6 and the second mixing cylinder 7 is opened, the iodine solution in the first mixing cylinder 6 and phenylsilane solution in the second mixing cylinder 7 flow into the stepped sleeve 25 through the flow guide pipe 24 and then directly fall into the mixing basin 33, in order to ensure the sealing effect of the connection between the flow guide pipe 24 and the stepped sleeve 25, a plurality of groove rings are formed at the periphery of the flow guide pipe 24, and sealing rings are sleeved in the groove rings, the sealing effect between the flow guide pipe 24 and the stepped sleeve 25 is ensured by the sealing rings, in the process, the flow meter 26 detects the amount of the iodine solution and phenylsilane solution flowing out of the stepped sleeve 25, after the required mass is reached, the second electromagnetic control valve 27 is closed, the flow meter 26 selects the coriolis mass flow meter, the rotating shaft 11 in the second step rotates, the stirring rib 34 is driven to rotate, the iodine solution and phenylsilane solution in the mixing basin 33 are stirred to obtain the mixed reaction solution;
step five, micro-reaction: the liquid outlet pipe 35 is communicated with the input end of an external water pump, the external water pump is communicated with the input end of the microchannel reactor, after the stirring in the fourth step is completed, the third electromagnetic control valve 36 is opened, the external water pump pumps the mixed reaction liquid into the microchannel reactor, and the reaction is continued for a set time in a room-temperature microchannel at 20 ℃ to obtain a reaction mixture;
step six, reduced pressure distillation: and (3) rectifying the reaction mixture in the step five under reduced pressure, and collecting a product with the fraction temperature of 35-40 ℃ under 20+/-3 mmHg to obtain the high-purity diiodosilane.
In this embodiment, the rotation of the driving motor 10 is used as driving power, so that not only can the rotation driving of the first mixing cylinder 6 and the second mixing cylinder 7 be realized, but also the rotation driving of the stirring rib rod 34 can be realized, so that the raw materials in the preparation process of diiodosilane can be pre-cooled conveniently, the sufficient and uniform mixing of different raw materials can be ensured, and convenience is provided for the preparation of high-purity diiodosilane.
Embodiment II,
This embodiment is a modification of the previous embodiment, and the preparation method of diiodosilane further includes the step four, in which when the iodine solution and the phenylsilane solution fall from the step sleeve 25, the iodine solution and the phenylsilane solution fall into the first diversion hole 31 on the plugging ring 29, in the process of rotating the rotating shaft 11 in the step two, the rotating shaft 11 drives the charging tray 30 to rotate, in the process of rotating the charging tray 30, when the second diversion hole 32 is communicated with the first diversion hole 31, the iodine solution and the phenylsilane solution pass through the second diversion hole 32 and fall into the mixing basin 33, and when the second diversion hole 32 is not communicated with the first diversion hole 31, the iodine solution and the phenylsilane solution are blocked by the charging tray 30, and no further blanking is performed.
The advantages of the embodiment over the first embodiment are: the intermittent blanking of the iodine solution and the phenylsilane solution can be realized, and the full mixing reaction of the iodine solution and the phenylsilane solution is effectively ensured.
Claims (10)
1. A preparation method of diiodosilane is characterized in that: the method specifically comprises the following steps:
step one, filling: after adding iodine and chloroform with set volume ratio into a first mixing cylinder (6) through a feeding pipe (37), plugging the feeding pipe (37), adding phenylsilane and ethyl acetate with set mass ratio into a second mixing cylinder (7) through another feeding pipe (37), and plugging the feeding pipe (37) to finish filling;
step two, premix: step one, in the process of filling, starting a driving assembly (9), driving the first mixing cylinder (6) and the second mixing cylinder (7) to rotate by the driving assembly (9) through a switching assembly (13), obtaining an iodine solution in the first mixing cylinder (6) after filling is completed for a set time, and obtaining a phenylsilane solution in the second mixing cylinder (7);
step three, precooling: the external refrigerating unit guides cold air into the mixing kettle (1) through the cold air inlet pipe (20) to refrigerate, and refrigerates the first mixing cylinder (6) and the second mixing cylinder (7) to realize precooling of iodine solution and phenylsilane solution;
step four, mixing reaction: cold air in the mixing kettle (1) is led into a mixing box (19) for refrigeration, a flow guide assembly (39) is opened, an iodine solution in a first mixing cylinder (6) and a phenylsilane solution in a second mixing cylinder (7) are led into a feeding assembly (28), the iodine solution and the phenylsilane solution are added into a mixing basin (33) by the feeding assembly (28), and after a driving assembly (9) is started, the iodine solution and the phenylsilane solution in the mixing basin (33) are stirred to obtain a mixed reaction solution;
step five, micro-reaction: after the stirring in the fourth step is completed, pumping the mixed reaction liquid into a microchannel reactor, and continuing to react in a microchannel at room temperature for a set time to obtain a reaction mixture;
step six, reduced pressure distillation: and (3) rectifying the reaction mixture in the step five under reduced pressure, and collecting a product with the fraction temperature of 35-40 ℃ under 20+/-3 mmHg to obtain the high-purity diiodosilane.
2. The method for preparing diiodosilane according to claim 1, wherein: the top cover of compounding cauldron (1) is equipped with shutoff lid (2), the bottom fixedly connected with of compounding cauldron (1) inner chamber keeps apart section of thick bamboo (3), fixedly mounted has division board (4) between the inner wall of a section of thick bamboo (3) and compounding cauldron (1), the quantity of division board (4) is provided with four, and four division board (4) interval evenly distributed is in the periphery of a section of thick bamboo (3), the top fixedly connected with carrier plate (5) of a section of thick bamboo (3), the bottom of carrier plate (5) is fixedly connected with the top of division board (4);
the first mixing barrel (6) and the second mixing barrel (7) are both provided with two, and the top of the carrier plate (5) is provided with assembly holes (8) matched with the two first mixing barrels (6) and the second mixing barrel (7).
3. The method for preparing diiodosilane according to claim 2, wherein: the utility model provides a drive assembly (9) is including driving motor (10), driving motor (10) fixed mounting is at the top of shutoff lid (2), driving motor (10) output runs through shutoff lid (2) and fixed mounting has pivot (11), support plate (5), isolation section of thick bamboo (3) and compounding cauldron (1) setting are run through in proper order to the bottom of pivot (11), the bottom fixed mounting of shutoff lid (2) has stirring frame (12), the quantity of stirring frame (12) is provided with four, and four stirring frames (12) cooperate with two first compounding section of thick bamboo (6) and second compounding section of thick bamboo (7) respectively and use.
4. A process for preparing diiodosilane according to claim 3, wherein: the switching subassembly (13) is including four tooth ring (14) and gear (15), gear (15) cover is established and fixed mounting is in the periphery of pivot (11), a plurality of spout (16) have been seted up to the inside of tooth ring (14), the periphery of first compounding section of thick bamboo (6) and second compounding section of thick bamboo (7) and the top fixed mounting that is located carrier plate (5) have a plurality of assembly strip (17), assembly strip (17) and spout (16) cooperate and use.
5. The method for preparing diiodosilane according to claim 2, wherein: the utility model discloses a mixing kettle, including compounding cauldron (1), cold air inlet pipe (20), communication hole (21) have been seted up on the surface of division board (4), through cold air pipe (23) intercommunication between the bottom of compounding cauldron (1) and mixing box (19) top fixed connection, cold air inlet pipe (20) intercommunication is fixed in the periphery of compounding cauldron (1), and cold air inlet pipe (20) set up in the below of carrier plate (5), be provided with first electromagnetic control valve (22) on cold air inlet pipe (20), communication hole (21) have been seted up on the surface of division board (4), between compounding cauldron (1) bottom and mixing box (19), and cold air pipe (23) set up the inside at compounding cauldron (18).
6. The method for preparing diiodosilane according to claim 5, wherein: the two diversion assemblies (39) comprise four diversion pipes (24), the four diversion pipes (24) are respectively communicated and fixed at the bottoms of the first mixing cylinder (6) and the second mixing cylinder (7), four step sleeves (25) are communicated at the bottom of the mixing kettle (1), and the bottom ends of the diversion pipes (24) penetrate through the mixing kettle (1) and are matched with the step sleeves (25);
the periphery of the step sleeve (25) is sequentially provided with a flowmeter (26) and a second electromagnetic control valve (27) from top to bottom.
7. The method for preparing diiodosilane according to claim 6, wherein: the utility model provides a reinforced subassembly (28) is including shutoff ring (29) and charging tray (30), the bottom of shutoff ring (29) and the top sliding contact of charging tray (30), the bottom of ladder sleeve pipe (25) runs through mixing box (19) and fixed mounting at the top of shutoff ring (29), first water conservancy diversion hole (31) with ladder sleeve pipe (25) intercommunication have been seted up to the bottom of shutoff ring (29), second water conservancy diversion hole (32) with first water conservancy diversion hole (31) looks adaptation have been seted up to the bottom of charging tray (30), and second water conservancy diversion hole (32) skew ladder sleeve pipe (25) set up.
8. The method for preparing diiodosilane according to claim 7, wherein: the mixing basin (33) is fixedly arranged at the bottom of an inner cavity of the mixing box (19) through a connecting rod, the feeding disc (30) is arranged at the top of the mixing basin (33), the bottom end of the rotating shaft (11) penetrates through the functional shell (18) and then penetrates through the mixing box (19), and the feeding disc (30) is sleeved and fixedly arranged on the periphery of the rotating shaft (11); the utility model discloses a mixing basin, including mixing box (19), pivot (11), inside fixed mounting that is located compounding basin (33) has a plurality of stirring rib pole (34), the bottom intercommunication of compounding basin (33) has drain pipe (35), the one end of drain pipe (35) runs through mixing box (19) and extends to the periphery of mixing box (19), and the surface of drain pipe (35) is provided with third electromagnetic control valve (36).
9. The method for preparing diiodosilane according to claim 2, wherein: the utility model discloses a sealing device for the high-pressure water heater, including blanking off cover (2), filling tube (37) are provided with four, and four filling tube (37) all run through the top that sets up at the shutoff lid (2), four the bottom of filling tube (37) runs through respectively in running through to two first compounding section of thick bamboo (6) and second compounding section of thick bamboo (7), the top threaded connection of filling tube (37) has lid (38).
10. Diiodosilane, characterized in that: made by the method of any of the preceding claims 1-9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310789246.0A CN116789140B (en) | 2023-06-29 | 2023-06-29 | Diiodosilane and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN109467090A (en) * | 2017-09-07 | 2019-03-15 | 江苏中能硅业科技发展有限公司 | The method of continuous production granular polycrystalline silicon |
| CN110606491A (en) * | 2019-06-20 | 2019-12-24 | 天津绿菱气体有限公司 | Preparation method of high-purity diiodosilane |
| WO2020062317A1 (en) * | 2018-09-29 | 2020-04-02 | 冯志容 | Material stirring device with filtering effect |
| WO2022016675A1 (en) * | 2020-07-24 | 2022-01-27 | 苏州波菲特新材料科技有限公司 | Ceramic converting agent, preparation method therefor and stirring device |
| CN114835126A (en) * | 2022-06-07 | 2022-08-02 | 安徽敦茂新材料科技有限公司 | Preparation method and device of diiodosilane |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109467090A (en) * | 2017-09-07 | 2019-03-15 | 江苏中能硅业科技发展有限公司 | The method of continuous production granular polycrystalline silicon |
| WO2020062317A1 (en) * | 2018-09-29 | 2020-04-02 | 冯志容 | Material stirring device with filtering effect |
| CN110606491A (en) * | 2019-06-20 | 2019-12-24 | 天津绿菱气体有限公司 | Preparation method of high-purity diiodosilane |
| WO2022016675A1 (en) * | 2020-07-24 | 2022-01-27 | 苏州波菲特新材料科技有限公司 | Ceramic converting agent, preparation method therefor and stirring device |
| CN114835126A (en) * | 2022-06-07 | 2022-08-02 | 安徽敦茂新材料科技有限公司 | Preparation method and device of diiodosilane |
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