CN220940632U - Cold hydrogenation cooling system - Google Patents
Cold hydrogenation cooling system Download PDFInfo
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- CN220940632U CN220940632U CN202322670067.3U CN202322670067U CN220940632U CN 220940632 U CN220940632 U CN 220940632U CN 202322670067 U CN202322670067 U CN 202322670067U CN 220940632 U CN220940632 U CN 220940632U
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- energy recoverer
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- 238000001816 cooling Methods 0.000 title claims abstract description 81
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 62
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 37
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000001257 hydrogen Substances 0.000 claims abstract description 33
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- 238000011084 recovery Methods 0.000 claims abstract description 30
- 238000005406 washing Methods 0.000 claims description 50
- 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 description 16
- 239000005049 silicon tetrachloride Substances 0.000 claims description 16
- 230000008016 vaporization Effects 0.000 claims description 16
- 239000006200 vaporizer Substances 0.000 claims description 13
- 238000009834 vaporization Methods 0.000 claims description 12
- 238000013021 overheating Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 230000000630 rising effect Effects 0.000 claims description 5
- 239000012530 fluid Substances 0.000 abstract description 21
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract description 9
- 229920005591 polysilicon Polymers 0.000 abstract description 9
- 238000012423 maintenance Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 43
- 238000000034 method Methods 0.000 description 16
- 230000008569 process Effects 0.000 description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000011863 silicon-based powder Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 4
- 239000005052 trichlorosilane Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 239000005046 Chlorosilane Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000005201 scrubbing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The utility model discloses a cold hydrogenation temperature-raising and lowering system, and relates to the technical field of polysilicon production. The heat energy recovery combination comprises a plurality of stages of heat energy recoverers which are sequentially connected, a shell side runner and a tube side runner for heat exchange are arranged in each stage of heat energy recoverer, the temperature of fluid in the shell side runner is smaller than that of fluid in the tube side runner, the fluid in the shell side runner and the fluid in the tube side runner exchange heat mutually so as to recycle heat of the temperature of the fluid in the tube Cheng Liudao, the fluid in the shell side runner is heated, the fluid in the tube side runner is cooled, and the heating, cooling and heat recycling of polysilicon cold hydrogenation are realized. The device is provided with a parking cooling combination independently, one end of the parking cooling combination is connected with a hydrogen conveying pipeline, the other end of the parking cooling combination is connected with a material heating line and a fluidized bed bottom end inlet, and low-temperature hydrogen is utilized to rapidly cool the fluidized bed so as to rapidly cool a cold hydrogenation parking, save cold hydrogenation maintenance time and reduce cold hydrogenation maintenance cost.
Description
Technical Field
The utility model relates to the technical field of polysilicon production, in particular to a cold hydrogenation temperature-raising and lowering system.
Background
At present, the technology adopted in the production of polysilicon in China is basically an improved Siemens method. The polysilicon produced by the technology accounts for more than 80% of the total national yield. An important element in the technology of the improved siemens process is cold hydrogenation. The cold hydrogenation is to mix and heat hydrogen and silicon tetrachloride, and to carry out endothermic reaction with silicon powder in a fluidized bed reactor with the temperature of 530 ℃ to 560 ℃ and the pressure of 2.5MPa to 3.0 MPa. The reaction requires the addition of a proportion of catalyst to increase conversion. And (3) carrying out heat recovery, dust removal, washing and condensation on the tail gas after the reaction to obtain a chlorosilane product, and finally, sending the chlorosilane product to a rectification process for further treatment. The unreacted hydrogen is compressed by a circulating hydrogen compressor and then recycled. The cold hydrogenation effectively converts silicon tetrachloride into trichlorosilane, solves the problem of closed cycle of chlorine element, reduces comprehensive power consumption for producing polysilicon, and is an important cost-reducing way for producing polysilicon by an improved Siemens method.
In the prior art, the patent with the publication number of CN115340095A discloses a cold hydrogenation heat energy recovery system and a cold hydrogenation heat energy recovery method, wherein the cold hydrogenation heat energy recovery system comprises a raw material gas preheating mechanism, a raw material gas mixing and vaporizing group, a mixed gas heating mechanism, a fluidized bed, a quenching tower and a rough separation tower; the raw material gas preheating mechanism is provided with a first shell-side runner and a first tube-side runner for heat exchange, and the mixed gas heating mechanism is provided with a second shell-side runner and a second tube-side runner for heat exchange; the inlet of the first tube side runner is connected with an air supply source, the outlet of the first tube side runner is connected with the inlet of the raw material gas mixing and vaporizing group, the outlet of the raw material gas mixing and vaporizing group is connected with the inlet of the second shell side runner, the outlet of the second shell side runner is connected with the gas inlet of the fluidized bed, the outlet of the fluidized bed is connected with the inlet of the second tube side runner, the inlet of the second tube side runner is connected with the inlet of the quenching tower, the outlet of the quenching tower is connected with the inlet of the first shell side, and the outlet of the first shell side is connected with the rough separation tower. The invention realizes cold hydrogenation heat energy recovery, reduces heat waste, and reduces energy loss and production cost.
The cold hydrogenation heat energy recovery system disclosed in the above patent has the following defects:
1. According to the scheme, the cold hydrogenation start-stop cooling time is not considered, three-stage heat exchange is simultaneously used, so that the cold hydrogenation stop cooling time is overlong, and the cold hydrogenation overhaul cost is increased.
Disclosure of utility model
In order to overcome the defects in the prior art, the utility model aims to provide a cold hydrogenation cooling system so as to solve the problems that the cooling time is too long and the cold hydrogenation maintenance cost is increased.
In order to achieve the above purpose, the present utility model adopts the technical scheme that:
A cold hydrogenation temperature-raising and reducing system comprises a mixer, a heat energy recovery combination, a fluidized bed, a washing tower combination, a vaporization and overheating combination and a stopping and temperature-lowering combination;
The inlet of the mixer is connected with a hydrogen conveying pipeline and a silicon tetrachloride conveying pipeline, the heat energy recovery combination comprises a plurality of stages of heat energy recoverers which are sequentially connected, a shell side runner and a tube side runner for heat exchange are arranged in each stage of heat energy recoverer, the shell side runners of the plurality of stages of heat energy recoverers form a material heating line, and the tube side runners form a material cooling line;
In the material temperature rising line, a shell-side runner inlet of a first-stage heat energy recoverer is connected with an outlet of a mixer, a shell-side runner outlet of a previous-stage heat energy recoverer is connected with a shell-side runner inlet of a next-stage heat energy recoverer, and a shell-side runner outlet of a final-stage heat energy recoverer is connected with a bottom inlet of a fluidized bed;
in the material cooling line, a tube side runner inlet of a final-stage heat energy recoverer is connected to a top end outlet of a fluidized bed, a tube side runner outlet of a rear-stage heat energy recoverer is connected to a tube side runner inlet of a front-stage heat energy recoverer, a tube side runner outlet of a second-stage heat energy recoverer is connected to a washing tower combination inlet, and the washing tower combination comprises a plurality of washing towers which are connected in sequence;
The vaporization overheating combination is arranged in the material heating line, one end of the stopping cooling combination is connected with the hydrogen conveying pipeline, and the other end of the stopping cooling combination is connected with the material heating line and the inlet at the bottom end of the fluidized bed.
Preferably, the heat energy recovery combination comprises a primary heat energy recoverer, a secondary heat energy recoverer, a tertiary heat energy recoverer and a quaternary heat energy recoverer;
The shell-side runner inlet of the primary heat energy recoverer is connected with the outlet of the mixer, the shell-side runner outlet of the primary heat energy recoverer is connected with the shell-side runner inlet of the secondary heat energy recoverer, the shell-side runner outlet of the secondary heat energy recoverer is connected with the shell-side runner inlet of the tertiary heat energy recoverer, the shell-side runner outlet of the tertiary heat energy recoverer is connected with the shell-side runner inlet of the quaternary heat energy recoverer, and the shell-side runner outlet of the quaternary heat energy recoverer is connected to the bottom inlet of the fluidized bed;
The top outlet of the fluidized bed is connected with the tube side runner inlet of the four-stage heat energy recoverer, the tube side runner outlet of the four-stage heat energy recoverer is connected with the tube side runner inlet of the three-stage heat energy recoverer, the tube side runner outlet of the three-stage heat energy recoverer is connected with the tube side runner inlet of the two-stage heat energy recoverer, and the tube side runner outlet of the two-stage heat energy recoverer is connected to the combined inlet of the washing tower.
Preferably, the vaporization overheating combination is arranged in a material heating line between a shell-side flow passage outlet of the primary heat energy recoverer and a shell-side flow passage inlet of the secondary heat energy recoverer, and comprises a vaporizer and a superheater;
The evaporator inlet is connected with the shell-side flow passage outlet of the primary heat energy recoverer, the evaporator outlet is connected with the superheater inlet, and the superheater outlet is connected with the shell-side flow passage inlet of the secondary heat energy recoverer.
Preferably, the four-stage heat energy recovery device further comprises an electric heater, wherein the shell side runner outlet of the four-stage heat energy recovery device is connected with the inlet of the electric heater, and the outlet of the electric heater is connected to the inlet at the bottom end of the fluidized bed.
Preferably, the parking cooling combination comprises a first heat exchanger and a second heat exchanger which are connected in parallel, the heat exchange temperature of the first heat exchanger is higher than that of the second heat exchanger, an inlet main pipe of the first heat exchanger and an inlet main pipe of the second heat exchanger are connected with a hydrogen conveying pipeline, and an outlet main pipe of the first heat exchanger and an outlet main pipe of the second heat exchanger are connected to an inlet at the bottom end of the fluidized bed.
Preferably, a first pipeline connected with the inlet and the outlet is arranged between the inlet and the outlet of the shell side runner of the three-stage heat energy recoverer, and a valve I is arranged on the first pipeline;
The outlet main pipes of the first heat exchanger and the second heat exchanger are connected with a second pipeline, the second pipeline is connected to the inlet of the shell side flow passage of the secondary heat energy recoverer, and a valve II is arranged on the second pipeline;
The hydrogen conveying pipeline is provided with a valve III for controlling materials to enter the mixer;
And a valve IV and a valve V are respectively arranged on the inlet branch pipes of the first heat exchanger and the second heat exchanger.
Preferably, the first heat exchanger is a circulating water heat exchanger, and the second heat exchanger is a 7 ℃ heat exchanger.
Preferably, the washing tower combination comprises a washing tower I and a washing tower II, wherein the bottom inlet of the washing tower I is connected with the tube side runner outlet of the secondary heat energy recoverer, the top outlet of the washing tower I is connected with the bottom inlet of the washing tower II, the top outlet of the washing tower II is connected to the tube side runner inlet of the primary heat energy recoverer, and the tube side runner outlet of the primary heat energy recoverer is connected to the downstream device.
The utility model has the beneficial effects that:
The utility model provides a cold hydrogenation cooling system, which comprises a plurality of stages of heat energy recoverers connected in sequence, wherein each stage of heat energy recoverer is internally provided with a shell-side runner and a tube-side runner for heat exchange, the temperature of fluid in the shell-side runner is lower than that of fluid in the tube-side runner, and the fluid in the shell-side runner and the fluid in the tube-side runner exchange heat with each other so as to recycle heat of the fluid in a tube Cheng Liudao, heat the fluid in the shell-side runner, and cool the fluid in the tube-side runner; the shell side flow channels of the heat energy recoverer form a material heating circuit, and the tube side flow channels form a material cooling circuit, so that the heating, cooling and heat recovery and utilization of polysilicon cold hydrogenation are realized.
The cold hydrogenation cooling system provided by the utility model is independently provided with the parking cooling combination, one end of the parking cooling combination is connected with the hydrogen conveying pipeline, the other end of the parking cooling combination is connected with the material heating line and the inlet at the bottom end of the fluidized bed, and the fluidized bed is rapidly cooled by utilizing low-temperature hydrogen and low-temperature materials in the material heating line so as to rapidly cool the cold hydrogenation parking, thereby saving cold hydrogenation overhaul time and reducing cold hydrogenation overhaul cost. The washing tower combination comprises a plurality of washing towers which are connected in sequence, the multi-stage washing effect is better, and the product quality is effectively improved.
Drawings
FIG. 1 is a schematic illustration of the present utility model;
FIG. 2 is a schematic view of the belt material of the present utility model;
Reference numerals:
1. A mixer; 2. a fluidized bed; 3. a primary heat energy recoverer; 4. a secondary heat energy recoverer; 5. a three-stage heat energy recoverer; 6. a four-stage thermal energy recoverer; 7. a vaporizer; 8. a superheater; 9. an electric heater; 10. a first heat exchanger; 11. a second heat exchanger; 12. a washing tower I; 13. a washing tower II; 14. a valve I; 15. a valve II; 16. a valve III; 17. a valve IV; 18. and a valve V.
Detailed Description
The conception, specific structure, and technical effects produced by the present utility model will be clearly and completely described below with reference to the embodiments and the drawings to fully understand the objects, features, and effects of the present utility model.
Example 1
A cold hydrogenation temperature-raising and lowering system, as shown in figures 1 and 2, comprises a mixer 1, a heat energy recovery combination, a fluidized bed 2, a washing tower combination, a vaporization and overheating combination and a stopping temperature-lowering combination.
The inlet of the mixer 1 is connected with a hydrogen conveying pipeline and a silicon tetrachloride conveying pipeline, the heat energy recovery combination comprises a plurality of stages of heat energy recoverers which are sequentially connected, a shell side runner and a tube side runner which are used for heat exchange are arranged in each stage of heat energy recoverer, the shell side runners of the plurality of stages of heat energy recoverers form a material heating circuit, and the tube side runners form a material cooling circuit.
In the material heating line, the shell-side runner inlet of the first-stage heat energy recoverer is connected with the outlet of the mixer 1, the shell-side runner outlet of the former-stage heat energy recoverer is connected with the shell-side runner inlet of the latter-stage heat energy recoverer, and the shell-side runner outlet of the final-stage heat energy recoverer is connected to the bottom inlet of the fluidized bed 2.
In the material cooling line, the tube side runner inlet of the final-stage heat energy recoverer is connected to the top end outlet of the fluidized bed 2, the tube side runner outlet of the rear-stage heat energy recoverer is connected with the tube side runner inlet of the front-stage heat energy recoverer, the tube side runner outlet of the second-stage heat energy recoverer is connected to the washing tower combination inlet, and the washing tower combination comprises a plurality of washing towers which are connected in sequence.
The vaporization overheating combination is arranged in the material heating line, one end of the stopping cooling combination is connected with the hydrogen conveying pipeline, and the other end is connected with the material heating line and the inlet at the bottom end of the fluidized bed 2. The side wall of the fluidized bed 2 is provided with a silica powder adding port.
In the embodiment, the mixer 1 is used for mixing the hydrogen and the silicon tetrachloride conveyed by the hydrogen conveying pipeline and the silicon tetrachloride conveying pipeline. The heat energy recovery combination is used for carrying out heat exchange on materials, heating or cooling the materials, and recycling heat. The fluidized bed 2 is used for reacting hydrogen, silicon tetrachloride and silicon powder to generate trichlorosilane. The washing tower combination is used for washing materials. The vaporization superheating combination is used for carrying out vaporization superheating on the mixed gas of hydrogen and silicon tetrachloride. The parking cooling combination is used for cold hydrogenation parking cooling.
In this embodiment, the heat energy recovery assembly includes several stages of heat energy recoverers connected in sequence, each stage of heat energy recoverer is provided with a shell-side runner and a tube-side runner for heat exchange, the temperature of fluid in the shell-side runner is smaller than that of fluid in the tube-side runner, the fluid in the shell-side runner and the fluid in the tube-side runner exchange heat with each other so as to recycle the heat of the fluid in the tube Cheng Liudao, heat the fluid in the shell-side runner, and cool the fluid in the tube-side runner; the shell side flow channels of the heat energy recoverer form a material heating circuit, and the tube side flow channels form a material cooling circuit, so that the heating, cooling and heat recovery and utilization of polysilicon cold hydrogenation are realized.
Example 2
This embodiment is further illustrated on the basis of example 1, as shown in fig. 1 and 2, the heat recovery assembly includes a primary heat energy recoverer 3, a secondary heat energy recoverer 4, a tertiary heat energy recoverer 5, and a quaternary heat energy recoverer 6.
The shell-side runner inlet of the primary heat energy recoverer 3 is connected with the outlet of the mixer 1, the shell-side runner outlet of the primary heat energy recoverer 3 is connected with the shell-side runner inlet of the secondary heat energy recoverer 4, the shell-side runner outlet of the secondary heat energy recoverer 4 is connected with the shell-side runner inlet of the tertiary heat energy recoverer 5, the shell-side runner outlet of the tertiary heat energy recoverer 5 is connected with the shell-side runner inlet of the quaternary heat energy recoverer 6, and the shell-side runner outlet of the quaternary heat energy recoverer 6 is connected to the bottom inlet of the fluidized bed 2.
The top end outlet of the fluidized bed 2 is connected with the tube side runner inlet of the four-stage heat energy recoverer 6, the tube side runner outlet of the four-stage heat energy recoverer 6 is connected with the tube side runner inlet of the three-stage heat energy recoverer 5, the tube side runner outlet of the three-stage heat energy recoverer 5 is connected with the tube side runner inlet of the two-stage heat energy recoverer 4, and the tube side runner outlet of the two-stage heat energy recoverer 4 is connected to the combined inlet of the washing tower.
In the embodiment, by arranging the four-stage heat energy recoverer in the form, the four-stage heat energy is recovered in a gradient way, so that the heat recovery rate is higher, and the power consumption is lower.
Example 3
This embodiment is further described on the basis of example 2, and as shown in fig. 1 and 2, the vaporization superheating combination is disposed in the material heating line between the shell-side flow channel outlet of the primary heat energy recoverer 3 and the shell-side flow channel inlet of the secondary heat energy recoverer 4, and includes a vaporizer 7 and a superheater 8.
The inlet of the vaporizer 7 is connected with the shell-side runner outlet of the primary heat energy recoverer 3, the outlet of the vaporizer 7 is connected with the inlet of the superheater 8, and the outlet of the superheater 8 is connected with the shell-side runner inlet of the secondary heat energy recoverer 4.
In this embodiment, the vaporizer 7 is used for vaporizing a mixed gas of hydrogen and silicon tetrachloride. The superheater 8 is used for reheating the mixed gas of the vaporizer 7 into superheated gas.
As shown in fig. 1 and 2, the fluidized bed further comprises an electric heater 9, wherein the shell-side runner outlet of the four-stage heat energy recoverer 6 is connected with the inlet of the electric heater 9, and the outlet of the electric heater 9 is connected with the inlet at the bottom end of the fluidized bed 2. The electric heater 9 is used for electrically heating the mixed gas of the hydrogen and the silicon tetrachloride.
Example 4
The embodiment is further described on the basis of embodiment 3, as shown in fig. 1 and 2, the shutdown cooling combination comprises a first heat exchanger 10 and a second heat exchanger 11 connected in parallel, the heat exchange temperature of the first heat exchanger 10 is greater than that of the second heat exchanger 11, inlet main pipes of the first heat exchanger 10 and the second heat exchanger 11 are connected with a hydrogen conveying pipeline, and outlet main pipes are connected to the inlet at the bottom end of the fluidized bed 2. The first heat exchanger 10 and the second heat exchanger 11 are used for exchanging heat for hydrogen, delivering the cooled hydrogen to the fluidized bed 2, and stopping the operation for cooling.
As shown in fig. 1 and 2, a first pipeline connecting the inlet and the outlet is arranged between the inlet and the outlet of the shell-side flow passage of the three-stage heat energy recoverer 5, and a valve i 14 is arranged on the first pipeline. The first pipe and the valve I14 thereon function as: the valve I14 is closed in the system heating process to speed up the heating, the valve I14 is fully opened in the system cooling process to speed up the cooling, the opening of the valve I14 is adjusted in the system operation process, and the shell side outlet temperature is adjusted.
As shown in fig. 1 and 2, the outlet main pipes of the first heat exchanger 10 and the second heat exchanger 11 are connected with a second pipeline, the second pipeline is connected to the inlet of the shell-side flow channel of the secondary heat energy recoverer 4, and a valve II 15 is arranged on the second pipeline. The second pipeline and the valve II 15 on the second pipeline have the following functions: and the valve II 15 is closed in the temperature rising process of the system to quicken the temperature rising speed, the valve II 15 is fully opened in the temperature reducing process of the system to quicken the temperature reducing speed, the opening of the valve II 15 is regulated in the running process of the system, and the shell side outlet temperature is regulated.
As shown in fig. 1 and 2, the hydrogen delivery line is provided with a valve iii 16 for controlling the material entering the mixer 1.
As shown in fig. 1 and 2, the inlet branch pipes of the first heat exchanger 10 and the second heat exchanger 11 are respectively provided with a valve iv 17 and a valve v 18, so that the hydrogen is controlled to enter the heat exchangers for heat exchange, and the temperature of the hydrogen is reduced.
As a preferred embodiment of the present example, the first heat exchanger 10 is a circulating water heat exchanger, and the second heat exchanger 11 is a 7 ℃ heat exchanger.
Example 5
This embodiment is further described on the basis of embodiment 4, as shown in fig. 1 and 2, the scrubber assembly includes a scrubber i 12 and a scrubber ii 13, the bottom inlet of the scrubber i 12 is connected to the tube side runner outlet of the second heat energy recovery device 4, the top outlet of the scrubber i 12 is connected to the bottom inlet of the scrubber ii 13, the top outlet of the scrubber ii 13 is connected to the tube side runner inlet of the first heat energy recovery device 3, and the tube side runner outlet of the first heat energy recovery device 3 is connected to the downstream device.
In this embodiment, the scrubber I12 is used for scrubbing and removing silicon powder, metal chloride and high boiling point in the gas entering the scrubber. The scrubber II 13 is used for further scrubbing the gas at the outlet of the scrubber I12.
As shown in figures 1 and 2, a spray liquid inlet pipe is arranged on the side wall at the top end of the washing tower II 13, a spray liquid conveying pipe is arranged between the bottom end of the washing tower II 13 and the side wall at the top end of the washing tower I12, and a downstream slag slurry conveying pipe is arranged at the bottom end of the washing tower I12.
For a better understanding of the present utility model, the following is a complete description of the principles of the utility model:
As shown in fig. 2, the hydrogen and the silicon tetrachloride conveyed by the hydrogen conveying pipeline and the silicon tetrachloride conveying pipeline enter the mixer 1 to be mixed, and the mixed materials enter the material heating line to be subjected to step heat exchange and heating.
Material heating circuit: the mixed material enters a shell side runner of the primary heat energy recoverer 3 from the mixer 1, and is subjected to primary heat exchange and temperature rise. The mixed material after the first heat exchange and temperature rise enters the vaporizer 7 for vaporization, and the vaporized mixed gas enters the superheater 8 for superheating. And then the mixed gas enters a shell-side runner of the secondary heat energy recoverer 4, and the mixed gas is subjected to secondary heat exchange and temperature rise. And the mixed gas after the second heat exchange and temperature rise enters a shell side runner of the three-stage heat energy recoverer 5, and the third heat exchange and temperature rise are carried out on the mixed gas. And the mixed gas after the third heat exchange and temperature rise enters a shell side runner of the four-stage heat energy recoverer 6, and the fourth heat exchange and temperature rise are carried out on the mixed gas. The mixed gas after the fourth heat exchange and temperature rise enters the electric heater 9 again, the mixed gas is electrically heated, and the mixed gas after the electric heating enters the fluidized bed 2 again.
Wherein the primary heat energy recoverer 3 exchanges heat from 50-60 ℃ to 100-120 ℃ for heating the mixture. The vaporizer 7 and the superheater 8 raise the temperature of the mixture from 100 to 120 ℃ to 150 to 170 ℃. The secondary heat energy recoverer 4 exchanges heat from 150-170 ℃ to 220-240 ℃ to heat the temperature of the mixed gas. The three-stage heat energy recoverer 5 exchanges heat from 220-240 ℃ to 310-330 ℃ for the temperature of the mixed gas. The temperature of the mixed gas is heat-exchanged and raised from 310-330 ℃ to 470-490 ℃ by the four-stage heat energy recoverer 6. The electric heater 9 increases the temperature of the mixed gas from 470-490 deg.c to 560 deg.c.
In the fluidized bed 2, silicon powder is introduced, the silicon powder reacts with high-temperature mixed gas (hydrogen and silicon tetrachloride), about 23% -35% of silicon tetrachloride reacts to generate trichlorosilane, and the high-temperature mixed gas such as trichlorosilane, unreacted silicon tetrachloride and hydrogen enters a material cooling line to perform gradient heat exchange and cooling.
Material cooling circuit: the high-temperature mixed gas enters a tube side runner of the four-stage heat energy recoverer 6 from the fluidized bed 2, and is subjected to primary heat exchange and temperature reduction. And the high-temperature mixed gas subjected to the first heat exchange and cooling enters a tube side runner of the three-stage heat energy recoverer 5, and the second heat exchange and cooling are performed on the high-temperature mixed gas. And the high-temperature mixed gas subjected to the second heat exchange and cooling enters a tube side flow passage of the secondary heat energy recoverer 4, and the third heat exchange and cooling are performed on the high-temperature mixed gas. And the high-temperature mixed gas subjected to the third heat exchange and cooling enters a washing tower I12 and a washing tower II 13 for washing, finally enters a tube pass runner of the primary heat energy recoverer 3 for the fourth heat exchange and cooling, and is conveyed to a downstream device. The liquid phase spray liquid enters a washing tower II 13 from the top, is sent to the top of a washing tower I12 from the bottom of the washing tower II 13, and is sent to slag discharge after coming out from the bottom of the washing tower I12.
The temperature of the high-temperature mixed gas is exchanged from 550 ℃ to 370-490 ℃ by the four-stage heat energy recoverer 6. The three-stage heat energy recoverer 5 exchanges heat from 370-390 ℃ to 300-320 ℃ to cool the temperature of the high-temperature mixed gas. The secondary heat energy recoverer 4 exchanges heat from 300-320 ℃ to 220-240 ℃ to cool the temperature of the high-temperature mixed gas. The temperature of the high-temperature mixed gas is reduced from 220-240 ℃ to 130-150 ℃ by the washing tower I12 and the washing tower II 13. The primary heat energy recoverer 3 exchanges heat from 130-150 ℃ to 80-100 ℃ to cool the temperature of the high-temperature mixed gas.
When the cold hydrogenation cooling system is operated for a period of time and is required to be stopped for maintenance, a stopping cooling process is carried out, and the method specifically comprises the following steps:
As shown in fig. 2, after the system enters a cooling program, firstly, a valve I14 is opened to bypass the three-stage heat energy recoverer 5 for cooling, the cooling speed is controlled to be 40-60 ℃/h, and when the cooling speed is lower than 40 ℃/h, a valve II 15 is opened to continue cooling the system. When the cooling speed of the system is lower than 40 ℃/h, the valve III 16 is closed, the valve IV 17 is opened, hydrogen enters the circulating water pipe Cheng Liudao, the hydrogen is cooled and then is introduced into the fluidized bed, and the inside of the fluidized bed is continuously cooled. When the cooling speed of the system is lower than 40 ℃/h, the valve IV 17 is closed, the valve V18 is opened, hydrogen enters a tube side flow passage of the 7 ℃ heat exchanger, the hydrogen is cooled and then is introduced into the fluidized bed, and the inside of the fluidized bed is continuously cooled until the cooling of the system is completed.
In the method, the valve I14 is opened, the bypass cooling is carried out on the three-stage heat energy recoverer 5, the cooling speed is controlled to be 60 ℃/h, and the specific flow direction of materials in the process is as follows: most of the low-temperature materials pass through a valve I14, and a small part of the materials pass through a three-stage heat energy recoverer 5 and pass through a bypass heat exchanger shell pass to achieve the purpose of cooling.
When the cooling speed is lower than 40 ℃, the valve II 15 is opened to continuously cool the system, and the specific flow direction of the materials in the process is as follows: most of unheated low-temperature materials directly enter the fluidized bed 2 through a valve II 15, and a small part of materials pass through the shell passes of the second-stage heat energy recoverer 4, the third-stage heat energy recoverer 5 and the fourth-stage heat energy recoverer 6 to realize system cooling.
The above cooling rate refers specifically to the bottom temperature of the fluidized bed 2. The step cooling method is adopted, so that the cooling speed is uniform, the cooling is faster, the parking maintenance time is effectively saved, and the cost is reduced.
In the utility model, the earlier stage of cooling is as follows: the temperature of the fluidized bed 2 is about 560 ℃, and materials with lower temperature are required to be heated to the temperature difference of about 100 ℃ with the fluidized bed 2 through the primary heat energy recoverer 3, the vaporizer 7, the superheater 8, the secondary heat energy recoverer 4, the quaternary heat energy recoverer 6 and the electric heater 9 because of higher temperature, and then the fluidized bed 2 is cooled, so that the problem that the equipment of the fluidized bed 2 is damaged due to the fact that low-temperature materials directly cool the high-temperature fluidized bed 2 is avoided. The temperature of the fluidized bed 2 at the initial stage of cooling is about 560 ℃, if the fluidized bed is cooled by cold materials, the cooling speed is more than 60 ℃ per hour, and other heat exchangers can be damaged.
Cooling medium term: when the temperature of the fluidized bed 2 is lower, the temperature difference between the material and the cooled material is smaller, after the cooling speed is lower than 40 ℃/h, the material with lower temperature does not need to be preheated, and directly spans the secondary heat energy recoverer 4, the tertiary heat energy recoverer 5, the quaternary heat energy recoverer 6 and the electric heater 9, and enters the fluidized bed 2 through the valve II 15 to cool the material, so that stable cooling is ensured.
And (3) cooling later stage: when the temperature of the fluidized bed 2 is lower than 250 ℃, cold materials directly cross the second-stage heat energy recoverer 4, the third-stage heat energy recoverer 5, the fourth-stage heat energy recoverer 6 and the electric heater 9, and when the cooling speed of the bottom of the fluidized bed 2 cannot meet the cooling speed of 40 ℃/h, the circulating water heat exchanger and the 7 ℃ heat exchanger are needed to be used in sequence (the cooling materials do not pass through the material heating line any more). Cooling the cold materials through the circulating water heat exchanger and the 7 ℃ heat exchanger, and cooling the fluidized bed 2 again until the temperature of the fluidized bed 2 is reduced to below 50 ℃, thereby completing the whole cooling process.
Above-mentioned lower cooling material of temperature of letting in proper order like this ensures that cooling early stage, middling, later stage cold material all can keep enough difference in temperature with fluidized bed 2, and the cooling rate can keep 40-60 ℃/h, has both shortened cooling time, also guarantees the safe and stable operation of equipment.
While the embodiments of the present utility model have been described in detail, the present utility model is not limited to the embodiments described above, and various equivalent modifications and substitutions can be made by those skilled in the art without departing from the spirit of the present utility model, and these are intended to be included in the scope of the present utility model as defined in the appended claims.
Claims (8)
1. The cold hydrogenation temperature-increasing and reducing system is characterized by comprising a mixer (1), a heat energy recovery combination, a fluidized bed (2), a washing tower combination, a vaporization and overheating combination and a stopping temperature-reducing combination;
The inlet of the mixer (1) is connected with a hydrogen conveying pipeline and a silicon tetrachloride conveying pipeline, the heat energy recovery combination comprises a plurality of stages of heat energy recoverers which are sequentially connected, a shell side runner and a tube side runner for heat exchange are arranged in each stage of heat energy recoverer, the shell side runners of the plurality of stages of heat energy recoverers form a material heating line, and the tube side runners form a material cooling line;
in the material heating line, a shell-side runner inlet of a first-stage heat energy recoverer is connected with an outlet of a mixer (1), a shell-side runner outlet of a previous-stage heat energy recoverer is connected with a shell-side runner inlet of a next-stage heat energy recoverer, and a shell-side runner outlet of a final-stage heat energy recoverer is connected to a bottom end inlet of a fluidized bed (2);
in the material cooling line, a tube side runner inlet of a final-stage heat energy recoverer is connected to a top end outlet of a fluidized bed (2), a tube side runner outlet of a rear-stage heat energy recoverer is connected to a tube side runner inlet of a front-stage heat energy recoverer, a tube side runner outlet of a second-stage heat energy recoverer is connected to a washing tower combination inlet, and the washing tower combination comprises a plurality of washing towers which are connected in sequence;
The vaporization overheating combination is arranged in the material heating line, one end of the stopping cooling combination is connected with the hydrogen conveying pipeline, and the other end of the stopping cooling combination is connected with the material heating line and the inlet at the bottom end of the fluidized bed (2).
2. Cold hydrogenation heat rising system according to claim 1, characterized in that the heat energy recovery combination comprises a primary heat energy recovery (3), a secondary heat energy recovery (4), a tertiary heat energy recovery (5) and a quaternary heat energy recovery (6);
The shell-side runner inlet of the primary heat energy recoverer (3) is connected with the outlet of the mixer (1), the shell-side runner outlet of the primary heat energy recoverer (3) is connected with the shell-side runner inlet of the secondary heat energy recoverer (4), the shell-side runner outlet of the secondary heat energy recoverer (4) is connected with the shell-side runner inlet of the tertiary heat energy recoverer (5), the shell-side runner outlet of the tertiary heat energy recoverer (5) is connected with the shell-side runner inlet of the quaternary heat energy recoverer (6), and the shell-side runner outlet of the quaternary heat energy recoverer (6) is connected to the bottom inlet of the fluidized bed (2);
The top outlet of the fluidized bed (2) is connected with the tube side runner inlet of the four-stage heat energy recoverer (6), the tube side runner outlet of the four-stage heat energy recoverer (6) is connected with the tube side runner inlet of the three-stage heat energy recoverer (5), the tube side runner outlet of the three-stage heat energy recoverer (5) is connected with the tube side runner inlet of the two-stage heat energy recoverer (4), and the tube side runner outlet of the two-stage heat energy recoverer (4) is connected to the combined inlet of the washing tower.
3. The cold hydrogenation temperature raising and reducing system according to claim 2, wherein the vaporization overheating combination is arranged in a material temperature raising line between a shell side runner outlet of the primary heat energy recoverer (3) and a shell side runner inlet of the secondary heat energy recoverer (4), and comprises a vaporizer (7) and a superheater (8);
The inlet of the vaporizer (7) is connected with the shell-side runner outlet of the primary heat energy recoverer (3), the outlet of the vaporizer (7) is connected with the inlet of the superheater (8), and the outlet of the superheater (8) is connected with the shell-side runner inlet of the secondary heat energy recoverer (4).
4. The cold hydrogenation temperature raising and lowering system according to claim 2, further comprising an electric heater (9), wherein the shell side runner outlet of the four-stage heat energy recoverer (6) is connected with the inlet of the electric heater (9), and the outlet of the electric heater (9) is connected with the inlet at the bottom end of the fluidized bed (2).
5. Cold hydrogenation temperature raising and lowering system according to claim 2, wherein the parking temperature lowering combination comprises a first heat exchanger (10) and a second heat exchanger (11) which are connected in parallel, the heat exchange temperature of the first heat exchanger (10) is higher than the heat exchange temperature of the second heat exchanger (11), an inlet main pipe of the first heat exchanger (10) and an inlet main pipe of the second heat exchanger (11) are connected with a hydrogen conveying pipeline, and an outlet main pipe is connected to the bottom inlet of the fluidized bed (2).
6. Cold hydrogenation temperature raising and lowering system according to claim 5, characterized in that a first pipeline connecting the inlet and the outlet is arranged between the inlet and the outlet of the shell side runner of the three-stage heat energy recoverer (5), and a valve I (14) is arranged on the first pipeline;
The outlet main pipes of the first heat exchanger (10) and the second heat exchanger (11) are connected with a second pipeline, the second pipeline is connected to the inlet of the shell side flow channel of the secondary heat energy recoverer (4), and a valve II (15) is arranged on the second pipeline;
the hydrogen conveying pipeline is provided with a valve III (16) for controlling materials to enter the mixer (1);
The inlet branch pipes of the first heat exchanger (10) and the second heat exchanger (11) are respectively provided with a valve IV (17) and a valve V (18).
7. Cold hydrogenation heat rising system according to claim 5, wherein the first heat exchanger (10) is a circulating water heat exchanger and the second heat exchanger (11) is a 7 ℃ heat exchanger.
8. The cold hydrogenation temperature raising and lowering system according to claim 2, wherein the washing tower combination comprises a washing tower I (12) and a washing tower II (13), wherein a bottom end inlet of the washing tower I (12) is connected with a tube side runner outlet of the secondary heat energy recoverer (4), a top end outlet of the washing tower I (12) is connected with a bottom end inlet of the washing tower II (13), a top end outlet of the washing tower II (13) is connected to a tube side runner inlet of the primary heat energy recoverer (3), and a tube side runner outlet of the primary heat energy recoverer (3) is connected to a downstream device.
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CN202322670067.3U CN220940632U (en) | 2023-10-07 | 2023-10-07 | Cold hydrogenation cooling system |
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