CN116282036B - Polysilicon cold hydrogenation catalyst recycling and separating equipment and polysilicon production system - Google Patents
Polysilicon cold hydrogenation catalyst recycling and separating equipment and polysilicon production system Download PDFInfo
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- CN116282036B CN116282036B CN202310102794.1A CN202310102794A CN116282036B CN 116282036 B CN116282036 B CN 116282036B CN 202310102794 A CN202310102794 A CN 202310102794A CN 116282036 B CN116282036 B CN 116282036B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 147
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 47
- 229920005591 polysilicon Polymers 0.000 title claims abstract description 44
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 238000004064 recycling Methods 0.000 title claims description 24
- 238000011084 recovery Methods 0.000 claims abstract description 184
- 239000002245 particle Substances 0.000 claims abstract description 52
- 238000000926 separation method Methods 0.000 claims abstract description 37
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 34
- 230000005389 magnetism Effects 0.000 claims abstract description 9
- 238000004891 communication Methods 0.000 claims description 12
- 230000007704 transition Effects 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 230000000903 blocking effect Effects 0.000 claims description 7
- 230000008602 contraction Effects 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- 239000012535 impurity Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 39
- 230000005291 magnetic effect Effects 0.000 description 20
- 238000005452 bending Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 229910003902 SiCl 4 Inorganic materials 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 3
- 238000010924 continuous production Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 229910003336 CuNi Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 208000012839 conversion disease Diseases 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 2
- 239000005052 trichlorosilane Substances 0.000 description 2
- 230000001960 triggered effect Effects 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- -1 Al 2O3 Substances 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 1
- 229910003910 SiCl4 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002907 paramagnetic material Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100001234 toxic pollutant Toxicity 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention discloses a polysilicon cold hydrogenation catalyst recovery separation device which comprises a recovery separator, wherein the recovery separator comprises a main pipeline, a first recovery branch pipe and a recovery magnet, the main pipeline comprises a horizontal pipe section and a vertical pipe section communicated with the horizontal pipe section, a port of the horizontal pipe section is connected with an air outlet of a fluidized bed reactor, a bottom port of the vertical pipe section is used as an outlet of silicon tetrachloride gas, one end of the first recovery branch pipe is communicated with a pipe body of the vertical pipe section, the other end of the first recovery branch pipe is used as an outlet of catalyst particles, the top of a joint of the first recovery branch pipe and the vertical pipe section is a first smooth curved surface, and the arrangement position of the recovery magnet is connected to the top of the first recovery branch pipe along the top of the horizontal pipe section and the first smooth curved surface. The polysilicon cold hydrogenation catalyst recovery and separation equipment can utilize magnetism to efficiently separate the catalyst, reduce the production cost and the impurity content of the product, thereby guaranteeing the purity and quality of the product.
Description
Technical Field
The invention belongs to the technical field of polysilicon production, and particularly relates to polysilicon cold hydrogenation catalyst recycling and separating equipment and a polysilicon production system.
Background
The Siemens method polysilicon production process is mainly realized by reducing trichlorosilane (SiHCl 3) vapor deposition silicon by utilizing hydrogen, and more than fifteen tons of silicon tetrachloride (SiCl 4).SiCl4 is a highly toxic pollutant and reacts with water vigorously) can be produced per ton of polysilicon produced, so that the Siemens method polysilicon production process is inconvenient for storage and transportation, and the hydrogenation of SiCl 4 into trichlorosilane (SiHCl 3) in the tail gas treatment process is the best solution at present for recycling.
The domestic enterprise SiCl 4 is mostly hydrogenated by adopting cold hydrogenation technology, namely SiCl 4 and silicon powder, hydrogen react at 470-550 ℃ under the action of a catalyst to generate SiHCl 3, namely:
SiCl 4+3Si+2H2→4SiHCl3. The catalyst used in the cold hydrogenation technology is mainly a transition metal catalyst represented by copper and nickel-based catalyst, but because high-temperature gas-solid three-phase reaction occurs in a fluidized bed, catalyst powder is generally easy to sinter and agglomerate, the contact efficiency of catalyst particles and silicon powder particles is low, the reaction conversion rate is low, and the catalyst is difficult to separate from air flow after the reaction, so that the catalyst is easy to be lost along with the air flow.
Currently, chinese patent application publication No. CN102814181a discloses CuNi alloy catalysts with good thermal stability; chinese patent application publication No. CN102114426a discloses catalysts using structural stabilizers such as Al 2O3、SiO2; the Chinese patent application with publication number of CN102350362A discloses a scheme for nanocrystallizing a CuNi alloy catalyst, so that the overall activity of the catalyst is effectively improved. Although the above patent more or less solves the problems of easy agglomeration and low reaction conversion rate, the existing catalyst design scheme still faces the problems of difficult separation from gas products and loss caused by gas flow entrainment, which not only reduces the catalytic efficiency, but also increases the production cost, further increases the impurity content of downstream products, and seriously affects the purity and quality of the final polysilicon product.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art, and provides a polysilicon cold hydrogenation catalyst recovery and separation device which can efficiently separate a catalyst by utilizing magnetism.
The invention provides a polysilicon cold hydrogenation catalyst recovery and separation device, which comprises a recovery separator, wherein the recovery separator comprises a main pipeline, a first recovery branch pipe and a recovery magnet, the main pipeline is a 90-degree bent pipeline and comprises a horizontal pipe section and a vertical pipe section communicated with the horizontal pipe section, and a port of the horizontal pipe section is connected with an air outlet of a fluidized bed reactor and is used for receiving silicon tetrachloride gas which is produced by the fluidized bed reactor and carries catalyst particles; the bottom port of a vertical pipe section is used as an outlet of silicon tetrachloride gas, one end of a first recovery branch pipe is communicated with a pipe body of the vertical pipe section, the other end of the first recovery branch pipe is used as an outlet of catalyst particles, the top of the joint of the first recovery branch pipe and the vertical pipe section is a first smooth curved surface, and the arrangement position of a recovery magnet is connected to the top of the first recovery branch pipe along the top of a horizontal pipe section and the first smooth curved surface and is used for guiding the catalyst particles to be discharged along the first recovery branch pipe by utilizing magnetism.
Preferably, the connection part between the first recovery branch pipe and the vertical pipe section is not completely communicated, the upper part of the connection part is provided with a communication port serving as a catalyst particle circulation through hole, and the lower part of the connection part is used as a blocking part for blocking the backflow of catalyst particles.
Preferably, the first recovery branch pipe is provided with two first high-pressure valves, and the two first high-pressure valves are arranged at the tail end of the first recovery branch pipe at intervals and used for forming a transition cabin isolated from the first recovery branch pipe and the external environment.
Preferably, the recovery separator further comprises a second recovery branch pipe, the recovery magnet is further arranged at the second recovery branch pipe, two branches are formed at the lower portion of the vertical pipe section, a bottom port of one vertical branch is used as an outlet of silicon tetrachloride gas, the other branch is the second recovery branch pipe, a port of the second recovery branch pipe is used as an outlet of catalyst particles remained in the silicon tetrachloride gas, the top of a joint of the second recovery branch pipe and the vertical pipe section is a second smooth curved surface, the recovery magnet is arranged at the second recovery branch pipe, and the arrangement position of the recovery magnet is connected to the top of the second recovery branch pipe along the side wall of the vertical pipe section above the second recovery branch pipe and the second smooth curved surface, so that the catalyst particles remained in the silicon tetrachloride gas are guided to be discharged along the second recovery branch pipe by magnetism.
Preferably, the port of the horizontal pipe section is smaller than the air outlet of the fluidized bed reactor, the horizontal pipe section and the vertical pipe section are connected through a flange, the port from the lower part to the bottom of the vertical pipe section is gradually contracted into an opening with the diameter consistent with the air outlet of the fluidized bed reactor, the contraction section is contracted to one side, one side of the contraction section is a vertical surface, the other side of the contraction section is an inclined surface, and the second recovery branch pipe is communicated with the inclined surface.
Preferably, the diameter of the communication opening between the second recovery branch pipe and the inclined plane is 0.5 to 1.0 times the length of the inclined plane.
Preferably, the second recovery branch pipe is provided with two second high-pressure valves, and the two second high-pressure valves are arranged at the tail end of the second recovery branch pipe at intervals and used for forming a transition cabin isolated from the second recovery branch pipe and the external environment.
Preferably, the recycling magnet comprises uniformly distributed magnets, the uniformly distributed magnets comprise a plurality of first electromagnet blocks, and the first electromagnet blocks are uniformly distributed along the arrangement positions of the recycling magnet.
Preferably, the uniformly distributed magnets are provided with two rows, and the first electromagnet blocks in the two rows are arranged in a staggered manner.
Preferably, the recycling magnet further comprises a rotary magnet, the rotary magnet comprises a rotating wheel and a plurality of second electromagnet blocks, each second electromagnet block is uniformly arranged on the rotating wheel around the axis of the rotating wheel, and the edge of the rotating wheel is tangent to the first smooth curved surface/the second smooth curved surface and rotates around the axis of the rotating wheel.
Preferably, the polysilicon cold hydrogenation catalyst recovery and separation device further comprises a shell, wherein the shell is covered outside the recovery separator, a plurality of cooling fans are arranged on the side wall of the shell, at least one cooling fan is located at the top of the shell and used as an air outlet fan, and at least one cooling fan is located in the middle of the shell and opposite to the recovery magnet and used as an air inlet fan.
The invention also provides a polysilicon production system, which comprises a fluidized bed reactor, a catalyst recovery tank, a raw material line and the polysilicon cold hydrogenation catalyst recovery and separation device, wherein the raw material line is connected with an inlet of the fluidized bed reactor, an air outlet of the fluidized bed reactor is connected with the polysilicon cold hydrogenation catalyst recovery and separation device, and an outlet of catalyst particles of the polysilicon cold hydrogenation catalyst recovery and separation device is connected with the catalyst recovery tank.
According to the polysilicon cold hydrogenation catalyst recovery and separation device, the main pipeline of the recovery separator is a 90-degree bent pipeline, so that the approximate flow direction of silicon tetrachloride gas also forms a bent streamline along the trend of the main pipeline. The first recovery branch pipe for recovering the catalyst particles is communicated with the vertical pipe section of the main pipeline and is inconsistent with the trend of the main pipeline, so that silicon tetrachloride gas and the trend of the catalyst particles can be separated.
The arrangement position of the recovery magnet is connected to the top of the first recovery branch pipe along the top of the horizontal pipe section and the first smooth curved surface for guiding the catalyst particles to be discharged along the first recovery branch pipe by magnetism. When silicon tetrachloride gas gets into the trunk line, at first reach the position of bending along horizontal pipe section, later turn into vertical pipe section along bending department, this in-process, catalyst particles in the silicon tetrachloride gas receive the magnetism effect of retrieving the magnet, can be close to towards the top of horizontal pipe section earlier automatically, later reach first smooth curved surface along bending department, because there is not the dog-ear between vertical pipe section and the first recovery branch pipe, catalyst particles can slide into in the first recovery branch pipe automatically under retrieving the effect of magnet, realize the recovery separation of catalyst, and silicon tetrachloride gas does not receive magnetic force to influence, can flow along the streamline of vertical pipe section originally.
Therefore, the equipment solves the problem that the existing high-activity polysilicon cold hydrogenation catalyst is easy to be entrained and lost by the airflow of the fluidized bed, utilizes the rule that catalyst particles have certain magnetism, applies a strong magnetic field at the air outlet of the fluidized bed reactor, efficiently adsorbs and separates the lost magnetic catalyst in the air outlet pipeline of the fluidized bed by adopting magnetic field force, induces the magnetic catalyst particles entrained in the airflow to deviate from the linear motion of the flow field, further enables the magnetic catalyst particles to enter a collecting and storing channel to complete the separation and recovery of the catalyst, achieves the purposes of recycling the catalyst, reducing the production cost and improving the purity of products, and effectively ensures the quality of subsequent products.
Drawings
FIG. 1 is a schematic diagram showing the structure of a polysilicon cold hydrogenation catalyst recovery and separation apparatus in example 1 of the present invention;
FIG. 2 is a schematic diagram of the structure of magnets uniformly distributed in a polysilicon cold hydrogenation catalyst recovery and separation apparatus according to example 1 of the present invention;
Fig. 3 is a schematic diagram of the structure of a rotary magnet in a polysilicon cold hydrogenation catalyst recovery and separation apparatus in example 1 of the present invention.
In the figure: 1. recovering the separator; 11. a main pipe; 111. a horizontal pipe section; 112. a vertical tube section; 113. a constriction section; 114. an inclined plane; 12. a first recovery branch pipe; 121. a first high pressure valve; 122. a communication port; 123. a blocking portion; 13. recovering the magnet; 131. uniformly distributed magnets; 132. a rotating magnet; 1321. a rotating wheel; 14. a second recovery branch pipe;
141. A second high pressure valve; 2. a fluidized bed reactor; 3. a housing; 31. a heat radiation fan;
4. a catalyst recovery tank.
Detailed Description
The following description of the embodiments of the present invention will be made more apparent, and the embodiments described in detail, but not necessarily all, in connection with the accompanying drawings. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
In the description of the present invention, it should be noted that, the terms "upper," "lower," and the like indicate an orientation or a positional relationship based on the orientation or the positional relationship shown in the drawings, and are merely for convenience and simplicity of description, and do not indicate or imply that the apparatus or element in question must be provided with a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
In the description of the present invention, the terms "first," "second," "third," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "connected," "configured," "mounted," "secured," and the like are to be construed broadly and may be either fixedly connected or detachably connected, or integrally connected, for example; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention can be understood by those skilled in the art according to the specific circumstances.
Example 1
As shown in fig. 1, the polysilicon cold hydrogenation catalyst recovery and separation device of the present embodiment comprises a recovery separator 1, wherein the recovery separator 1 comprises a main pipe 11, a first recovery branch pipe 12 and a recovery magnet 13, the main pipe 11 is a 90 ° bent pipe, and comprises a horizontal pipe section 111 and a vertical pipe section 112 communicated with the horizontal pipe section 111, and a port of the horizontal pipe section 111 is connected with an air outlet of a fluidized bed reactor 2 and is used for receiving silicon tetrachloride gas carrying catalyst particles produced by the fluidized bed reactor 2; the bottom port of the vertical pipe section 112 is used as an outlet of silicon tetrachloride gas, and the general flow direction of the silicon tetrachloride gas also forms a bending streamline along the trend of the main pipeline 11.
One end of the first recovery branch pipe 12 is communicated with the pipe body of the vertical pipe section 112, and the other end is used as an outlet of catalyst particles, namely, the trend of the first recovery branch pipe 12 for recovering the catalyst particles is not consistent with that of the main pipe 11, so that silicon tetrachloride gas and the trend of the catalyst particles can be separated. In this embodiment, the angle between the first recovery branch pipe 12 and the vertical pipe section 112 may be set to 10 ° to 80 °. The top of the junction of the first recovery branch pipe 12 and the vertical pipe section 112 is a first smooth curved surface, and the recovery magnet 13 is arranged along the top of the horizontal pipe section 111, and the first smooth curved surface is joined to the top of the first recovery branch pipe 12 for magnetically guiding the catalyst particles to be discharged along the first recovery branch pipe 12.
When silicon tetrachloride gas enters the main pipeline 11, firstly, the silicon tetrachloride gas reaches a bending position along the horizontal pipe section 111, then turns into the vertical pipe section 112 along the bending position, in the process, catalyst particles in the silicon tetrachloride gas are automatically close to the top of the horizontal pipe section 111 under the magnetic action of the recovery magnet 13, then reach a first smooth curved surface along the bending position, and because no bending angle exists between the vertical pipe section 112 and the first recovery branch pipe 12, the catalyst particles automatically slide into the first recovery branch pipe 12 under the action of the recovery magnet to realize recovery and separation of the catalyst, and the silicon tetrachloride gas is not influenced by magnetic force and flows out along the streamline of the original vertical pipe section 112.
Therefore, the equipment solves the problem that the existing high-activity polysilicon cold hydrogenation catalyst is easy to be entrained and lost by the airflow of the fluidized bed, utilizes the rule that catalyst particles have certain magnetism, applies a strong magnetic field at the air outlet of the fluidized bed reactor 2, efficiently adsorbs and separates the lost magnetic catalyst in the air outlet pipeline of the fluidized bed by adopting magnetic field force, induces the magnetic catalyst particles entrained in the airflow to deviate from the linear motion of the flow field, and further enables the magnetic catalyst particles to enter a collecting and storing channel to finish the separation and recovery of the catalyst, thereby achieving the purposes of recycling the catalyst, reducing the production cost and improving the purity of products and effectively ensuring the quality of subsequent products. The catalyst in this embodiment is a magnetic catalyst, and the magnetic catalyst is typically a ferromagnetic catalyst containing a material such as Ni, co, or Fe, or a catalyst containing a paramagnetic material such as NiCl 2、FeCl2.
In this embodiment, in order to ensure that the recovered catalyst transported into the first recovery branch pipe 12 is not carried back to the main pipe 11 again by the turbulence of the air flow, the junction between the first recovery branch pipe 12 and the vertical pipe section 112 is not completely through, the upper part of the junction is provided with a communication port 122 serving as a catalyst particle flow through hole, the lower part is provided with a blocking part 123 for blocking the backflow of the catalyst particles, and the vertical height from the first smooth curved surface to the lower edge of the communication port 122 is 0.1 to 0.5 times the diameter of the first recovery branch pipe 12. The catalyst particles flow along the top wall of the pipe toward the first recovery branch pipe 12 due to the magnetic field, so that the catalyst particles in the upper communication port do not block the catalyst from entering, but when the catalyst particles in the first recovery branch pipe 12 tend to flow backward, they cannot flow backward from the communication port due to being deposited at the bottom of the pipe. The communication port can be directly formed on the pipe wall of the vertical pipe section 112 according to the required size when two pipes are connected, or can be formed by completely communicating and then plugging, and the shape of the opening can be rectangular, semicircular and semi-elliptical according to the requirements.
In this embodiment, two first high-pressure valves 121 are disposed on the first recovery branch pipe 12, and the two first high-pressure valves 121 are disposed at intervals at the end of the first recovery branch pipe 12, so as to form a transition cabin isolated from the first recovery branch pipe 12 and the external environment.
The two first high-pressure valves 121 can be used for discharging the recovered catalyst in continuous production, when the first valves are opened, the catalyst cannot directly flow out, silicon tetrachloride gas cannot leak, after the catalyst enters the transition cabin, the first valves are closed, the second valves are opened, and the catalyst in the transition cabin can flow out, so that the gas inlet is not required to be stopped in the catalyst discharging process, the shutdown is not required, and continuous production can be realized.
In this embodiment, the recovery magnet 13 adopts an electromagnet with an external power supply to generate magnetic force, and plays a role in adsorbing, guiding and transmitting catalyst particles when magnetic, and the catalyst particles can be freely desorbed when non-magnetic, so that the catalyst can be conveniently collected and the tube wall can be conveniently cleaned.
When the catalyst recycling device is used, the power supply of the recycling magnet 13 can be periodically turned off, then the first high-pressure valve 121 is turned on, the first high-pressure valve 121 is turned off after the collected catalyst enters the transition cabin, the power supply of the recycling magnet 13 is turned on, then the second high-pressure valve 121 is turned on, the recycled catalyst is discharged, and recycling separation of the catalyst is completed.
The material height sensor and the alarm can be arranged on the first recovery branch pipe 12, and along with the increasing of the catalyst amount recovered in the first recovery branch pipe 12, the material height sensor can send a signal to the alarm after being triggered, and the alarm can give out prompts such as flashing, buzzing and vibration to indicate that the recovered catalyst needs to be discharged. Preferably, the material level sensor may be further coupled to a controller, and when the catalyst recovery amount reaches the target level in the first recovery branch pipe 12, a signal is sent to the controller, and the controller controls the orderly opening and closing of the two first high-pressure valves 121, so as to automatically complete the discharge of the catalyst.
In this embodiment, the material height sensor, the alarm, the controller and the like all belong to conventional devices on the market, the setting positions of the conventional devices can be selected according to needs, and the specific structure and principle of the conventional devices are not described herein.
In this embodiment, the recovery separator 1 further includes a second recovery branch pipe 14, the recovery magnet 13 is further disposed at the second recovery branch pipe 14, the lower portion of the vertical pipe section 112 forms two branches, wherein a bottom port of one of the vertical branches is used as an outlet of silicon tetrachloride gas, the other branch is the second recovery branch pipe 14, a port of the second recovery branch pipe 14 is used as an outlet of catalyst particles remained in the silicon tetrachloride gas, a top of a junction of the second recovery branch pipe 14 and the vertical pipe section 112 is a second smooth curved surface, and the recovery magnet 13 disposed at the second recovery branch pipe 14 is disposed at a position along a sidewall of the vertical pipe section 112 above the second recovery branch pipe 14 and the second smooth curved surface is connected to the top of the second recovery branch pipe 14 for magnetically guiding the catalyst particles remained in the silicon tetrachloride gas to be discharged along the second recovery branch pipe 14. In this embodiment, the angle between the second recovery branch pipe 14 and the vertical pipe section 112 may be set to 10 ° to 80 °.
In this embodiment, the first smooth curved surface and the second smooth curved surface may be obtained by polishing after welding, so as to achieve the effect of smooth connection between pipe sections.
The recovery process of the second recovery branch pipe 14 is basically identical to that of the first recovery branch pipe 12, but is arranged below the silicon tetrachloride gas flow line, and the arrangement mode realizes 'two-stage' separation and collection of the catalyst, and when the first recovery branch pipe 12 does not completely separate the catalyst particles, the residual catalyst particles in the silicon tetrachloride gas can be recovered by the second recovery branch pipe 14.
In this embodiment, the port of the horizontal pipe section 111 is smaller than the gas outlet of the fluidized bed reactor 2, and the two are connected by a flange, i.e. the connection between the gas outlet of the fluidized bed reactor 2 and the main pipe 11 is provided with a "sudden expansion" of the flow section, and the "sudden expansion" structure increases the turbulence degree of the outlet gas and simultaneously reduces the gas flow velocity, so as to enhance the effect of the electromagnetic field on the entrained catalyst particles.
While the lower to bottom port of the vertical tube section 112 gradually narrows to an opening of a diameter consistent with the gas outlet of the fluidized bed reactor 2 to reduce the impact of the application of the present apparatus on other production sections. And the shrinkage section 113 shrinks to one side, so that one side of the shrinkage section 113 is a vertical surface, the other side is an inclined surface 114, silicon tetrachloride gas is discharged to an outlet along the shrinkage section 113, and the second recovery branch pipe 14 is communicated with the inclined surface 114, so that catalyst particles generate streamline different from the silicon tetrachloride gas under the influence of a magnetic field and finally flow into the second recovery branch pipe 14 to realize recovery and utilization. In this embodiment, the angle between the inclined surface 114 and the horizontal plane is preferably in the range of 30 ° to 80 °.
In this embodiment, the diameter of the communication opening between the second recovery branch pipe 14 and the inclined surface 114 is 0.5 to 1.0 times the length of the inclined surface 114.
In this embodiment, two second high-pressure valves 141 are disposed on the second recovery branch pipe 14, and the two second high-pressure valves 141 are disposed at intervals at the end of the second recovery branch pipe 14, so as to form a transition cabin isolated from the second recovery branch pipe 14 and the external environment.
And in the same way, the space between the two valves is used as a transition cabin, the gas is not required to be stopped in the catalyst discharging process, and the stop is not required, so that continuous production can be realized. When the catalyst recycling device is used, the power supply of the recycling magnet 13 is periodically turned off, then the first high-pressure valve 141 is turned on, after the collected catalyst enters the transition cabin, the second high-pressure valve 141 is turned off, the power supply of the recycling magnet 13 is turned on, then the second high-pressure valve 141 is turned on, the recycled catalyst is discharged, and recycling separation of the catalyst is completed.
The second recovery branch pipe 14 may be provided with a material height sensor and an alarm, and as the amount of catalyst recovered in the second recovery branch pipe 14 increases, the material height sensor may send a signal to the alarm after being triggered, and the alarm may give out a prompt such as a flash, a buzzer, a vibration, etc., to indicate that the recovered catalyst needs to be discharged. Preferably, the material level sensor may be further coupled to a controller, and when the catalyst recovery amount reaches the target level in the second recovery branch pipe 14, a signal is sent to the controller, and the controller controls the orderly opening and closing of the two second high-pressure valves 141, so as to automatically complete the discharge of the catalyst.
In this embodiment, the material height sensor, the alarm, the controller and the like all belong to conventional devices on the market, the setting positions of the conventional devices can be selected according to needs, and the specific structure and principle of the conventional devices are not described herein.
In this embodiment, the recovery magnet 13 includes a uniform distribution magnet 131, and as shown in fig. 2, the uniform distribution magnet 131 includes a plurality of first electromagnet blocks, each of which is uniformly arranged along the arrangement position of the recovery magnet 13. In this embodiment, the uniformly distributed magnets 131 are provided with two rows, and the first electromagnet blocks in the two rows are arranged in a staggered manner. So as to completely cover the streamline of the catalyst along the pipe wall and ensure the sufficient adsorption effect.
In this embodiment, the recovery magnet 13 further includes two rotating magnets 132, as shown in fig. 3, the rotating magnets 132 include a rotating wheel 1321 and a plurality of second electromagnet blocks, each of which is uniformly arranged on the rotating wheel 1321 around the axis of the rotating wheel 1321, and the edges of the rotating wheels 1321 of the two rotating magnets 132 are tangent to the first smooth curved surface and the second smooth curved surface and revolve around their own axes. In order to avoid interference, the uniformly distributed magnets 131 are disconnected at the tangent position of the rotary magnet 132 and the curved surface, the rotary magnet 132 is driven to rotate by an externally connected gear motor, and along with the rotation of the plurality of second electromagnet blocks, the catalyst pre-adsorbed on the main pipeline 11 is guided to enter the first recovery branch pipe 12 and the second recovery branch pipe 14 from the main pipeline 11 and is discharged.
In this embodiment, the apparatus further includes a housing 3, the housing 3 is covered outside the recovery separator 1, a plurality of cooling fans 31 are disposed on a side wall of the housing 3, at least one cooling fan 31 is located at a top of the housing 3, and is used as an air outlet fan, at least one cooling fan 31 is located in a middle of the housing 3, opposite to the position of the recovery magnet 13, and is used as an air inlet fan, and each fan is combined in the housing 3 to perform ventilation, heat dissipation and temperature reduction, so as to ensure safe operation of the apparatus. A plurality of transparent observation windows can be further arranged on the shell 3, so that a worker can conveniently check the internal condition of the equipment.
Example 2
The polycrystalline silicon production system of the embodiment comprises a fluidized bed reactor 2, wherein the fluidized bed reactor 2 is used for an inter-cooling hydrogenation catalytic reaction process in polycrystalline silicon production, silicon tetrachloride gas flows upwards from the bottom in production, solid particles such as a catalyst and the like move randomly in the reactor, a gas outlet is arranged at the top of the reactor, and a pipeline for conveying the gas is connected.
The polysilicon production system further comprises a catalyst recovery tank 4, a raw material line and a polysilicon cold hydrogenation catalyst recovery and separation device in the embodiment 1, wherein the raw material line is connected with an inlet of the fluidized bed reactor 2, an air outlet of the fluidized bed reactor 2 is connected with the polysilicon cold hydrogenation catalyst recovery and separation device, and an outlet of catalyst particles of the polysilicon cold hydrogenation catalyst recovery and separation device is connected with the catalyst recovery tank 4.
It is to be understood that the above embodiments are merely illustrative of the application of the principles of the present invention, but not in limitation thereof. Various modifications and improvements may be made by those skilled in the art without departing from the spirit and substance of the invention, and are also considered to be within the scope of the invention.
Claims (11)
1. A polysilicon cold hydrogenation catalyst recovery and separation device is characterized in that: comprises a recovery separator (1), wherein the recovery separator (1) comprises a main pipeline (11), a first recovery branch pipe (12) and a recovery magnet (13),
The main pipeline (11) is a 90-degree bent pipeline and comprises a horizontal pipe section (111) and a vertical pipe section (112) communicated with the horizontal pipe section (111), wherein a port of the horizontal pipe section (111) is connected with an air outlet of the fluidized bed reactor (2) and is used for receiving silicon tetrachloride gas which is produced by the fluidized bed reactor (2) and carries catalyst particles; the bottom port of the vertical pipe section (112) is used as an outlet of silicon tetrachloride gas,
One end of the first recovery branch pipe (12) is communicated with the pipe body of the vertical pipe section (112), the other end is used as an outlet of catalyst particles,
The top of the joint of the first recovery branch pipe (12) and the vertical pipe section (112) is a first smooth curved surface, the arrangement position of the recovery magnet (13) is connected to the top of the first recovery branch pipe (12) along the top of the horizontal pipe section (111), and the first smooth curved surface is used for guiding catalyst particles to be discharged along the first recovery branch pipe (12) by magnetism;
the recovery separator (1) further comprises a second recovery branch pipe (14), the recovery magnet (13) is further arranged at the second recovery branch pipe (14),
The lower part of the vertical pipe section (112) forms two branches, wherein the bottom port of one vertical branch is used as an outlet of silicon tetrachloride gas, the other branch is a second recovery branch pipe (14), the port of the second recovery branch pipe (14) is used as an outlet of catalyst particles remained in the silicon tetrachloride gas,
The top of the joint of the second recovery branch pipe (14) and the vertical pipe section (112) is a second smooth curved surface,
The recycling magnet (13) is arranged at the second recycling branch pipe (14) and is connected to the top of the second recycling branch pipe (14) along the side wall of the vertical pipe section (112) above the second recycling branch pipe (14) and the second smooth curved surface, so as to magnetically guide the remained catalyst particles in the silicon tetrachloride gas to be discharged along the second recycling branch pipe (14).
2. The polysilicon cold hydrogenation catalyst recovery and separation apparatus according to claim 1, wherein: the joint between the first recovery branch pipe (12) and the vertical pipe section (112) is not completely communicated, the upper part of the joint is provided with a communication port (122) serving as a catalyst particle circulation through hole, and the lower part of the joint is used as a blocking part (123) for blocking the backflow of catalyst particles.
3. The polysilicon cold hydrogenation catalyst recovery and separation apparatus according to claim 1, wherein: the first recovery branch pipe (12) is provided with two first high-pressure valves (121), and the two first high-pressure valves (121) are arranged at the tail end of the first recovery branch pipe (12) at intervals and are used for forming a transition cabin isolated from the first recovery branch pipe (12) and the external environment.
4. The polysilicon cold hydrogenation catalyst recovery and separation apparatus according to claim 1, wherein: the port of the horizontal pipe section (111) is smaller than the air outlet of the fluidized bed reactor (2), the horizontal pipe section and the air outlet are connected through a flange,
The lower part of the vertical pipe section (112) gradually contracts to the bottom port to form an opening with the diameter consistent with the air outlet of the fluidized bed reactor (2), the contraction section (113) contracts to one side, one side of the contraction section (113) is a vertical surface, the other side of the contraction section is an inclined surface (114), and the second recovery branch pipe (14) is communicated with the inclined surface (114).
5. The polysilicon cold hydrogenation catalyst recovery and separation apparatus according to claim 4, wherein: the diameter of the communication opening between the second recovery branch pipe (14) and the inclined plane (114) is 0.5-1.0 times the length of the inclined plane (114).
6. The polysilicon cold hydrogenation catalyst recovery and separation apparatus according to claim 1, wherein: the second recovery branch pipe (14) is provided with two second high-pressure valves (141), and the two second high-pressure valves (141) are arranged at the tail end of the second recovery branch pipe (14) at intervals and are used for forming a transition cabin isolated from the second recovery branch pipe (14) and the external environment.
7. The polysilicon cold hydrogenation catalyst recovery and separation apparatus according to claim 1, wherein: the recycling magnet (13) comprises uniformly distributed magnets (131), each uniformly distributed magnet (131) comprises a plurality of first electromagnet blocks, and the first electromagnet blocks are uniformly distributed along the arrangement position of the recycling magnet (13).
8. The polysilicon cold hydrogenation catalyst recovery and separation apparatus as set forth in claim 7, wherein: the uniformly distributed magnets (131) are provided with two rows, and the first electromagnet blocks in the two rows are arranged in a staggered manner.
9. The polysilicon cold hydrogenation catalyst recovery and separation apparatus as set forth in claim 7, wherein: the recovery magnet (13) further comprises a rotary magnet (132), the rotary magnet (132) comprises a rotating wheel (1321) and a plurality of second electromagnet blocks, each second electromagnet block is uniformly arranged on the rotating wheel (1321) around the axis of the rotating wheel (1321),
The edge of the runner (1321) is tangent to the first smooth curved surface/the second smooth curved surface and revolves around its own axis.
10. The polysilicon cold hydrogenation catalyst recovery and separation apparatus according to claim 1, wherein: also comprises a shell (3), the shell (3) is covered outside the recovery separator (1),
A plurality of cooling fans (31) are arranged on the side wall of the shell (3), at least one cooling fan (31) is positioned at the top of the shell (3) and used as an air outlet fan, and at least one cooling fan (31) is positioned in the middle of the shell (3) and is opposite to the recovery magnet (13) in position and used as an air inlet fan.
11. A polycrystalline silicon production system, includes fluidized bed reactor (2), catalyst recovery jar (4) and former material line, its characterized in that: further comprising a polysilicon cold hydrogenation catalyst recovery separation apparatus as set forth in any one of claims 1 to 10,
The raw material line is connected with an inlet of the fluidized bed reactor (2), an air outlet of the fluidized bed reactor (2) is connected with the polysilicon cold hydrogenation catalyst recovery and separation device, and an outlet of catalyst particles of the polysilicon cold hydrogenation catalyst recovery and separation device is connected with the catalyst recovery tank (4).
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| CN101941702A (en) * | 2010-09-08 | 2011-01-12 | 洛阳晶辉新能源科技有限公司 | Method for producing trichlorosilane by converting silicon tetrachloride |
| CN114620731A (en) * | 2020-12-14 | 2022-06-14 | 新疆新特晶体硅高科技有限公司 | Recovery method and recovery device for reduction tail gas of polycrystalline silicon |
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| CN101125858B (en) * | 2007-09-05 | 2011-04-13 | 青岛科技大学 | Method for directly reclaiming catalyst of organic silicon monomer fluidized bed reactor and device thereof |
| CN110078080B (en) * | 2019-04-26 | 2022-09-02 | 天津科技大学 | Chlorosilane high-boiling-point substance recovery process combining slag slurry treatment and cracking reaction |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101941702A (en) * | 2010-09-08 | 2011-01-12 | 洛阳晶辉新能源科技有限公司 | Method for producing trichlorosilane by converting silicon tetrachloride |
| CN114620731A (en) * | 2020-12-14 | 2022-06-14 | 新疆新特晶体硅高科技有限公司 | Recovery method and recovery device for reduction tail gas of polycrystalline silicon |
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