CN217895154U - Trichlorosilane cold hydrogenation production system - Google Patents
Trichlorosilane cold hydrogenation production system Download PDFInfo
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- CN217895154U CN217895154U CN202221949434.2U CN202221949434U CN217895154U CN 217895154 U CN217895154 U CN 217895154U CN 202221949434 U CN202221949434 U CN 202221949434U CN 217895154 U CN217895154 U CN 217895154U
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Abstract
The utility model discloses a trichlorosilane cold hydrogenation production system, which belongs to the field of polysilicon energy saving and consumption reduction production. The device comprises an electric heater, a fluidized bed reactor, a first-stage heat exchanger, a second-stage heat exchanger and a separator, wherein the separator is connected with a washing tower, a continuous passage for synthesizing and purifying trichlorosilane is formed among the electric heater, the fluidized bed reactor, the first-stage heat exchanger, the second-stage heat exchanger, the separator and the washing tower, a mixed gas pipe is connected with a high-purity hydrogen chloride inlet pipe I, a mixed gas pipe is connected with a high-purity hydrogen chloride inlet pipe II, a conveying pipe is connected with a high-purity hydrogen chloride inlet pipe III, and the temperature in the fluidized bed is improved through exothermic reaction caused by adding high-purity hydrogen chloride, so that the reaction quality is improved; and unreacted silicon powder in the mixed gas is consumed, so that the efficiency of subsequent separation and purification is ensured.
Description
Technical Field
The utility model relates to a trichlorosilane cold hydrogenation production system, which belongs to the field of polysilicon energy-saving and consumption-reducing production.
Background
At present, the cold hydrogenation process mainly utilizes vaporized silicon tetrachloride to mix with hydrogen to form mixed gas, the mixed gas is heated by an electric heater, meanwhile, silicon powder in a furnace is relatively uniformly suspended in a fluidized bed through a distributor, the heated mixed gas reacts with the silicon powder under the conditions of 2.55-3.0Mpa and 550-560 ℃ to generate mixed gas containing trichlorosilane, dichlorosilane and silicon tetrachloride (fine silicon powder is also mixed in the mixed gas), the mixed gas is dedusted by a primary cyclone separator, dedusted by a secondary cyclone separator and washed by a washing tower, and then the mixed gas enters a condensing system to be cooled and cooled to obtain chlorosilane product liquid, and the related main reaction is as follows: 3SiCl 4 +Si+2H 2 =4SiHCl 3 -Q (endothermic reaction).
The reaction temperature in the fluidized bed is maintained by mainly heating and maintaining the reaction temperature by an electric heater, but the power consumption cost is too high, and the requirements of the energy-saving and emission-reducing production process are not met.
In addition, the mixed gas outlet end on the fluidized bed is a two-stage heat exchanger, and the first-stage cyclone separator and the second-stage cyclone separator are arranged at the rear end of the two-stage heat exchanger. The first grade heat exchanger is around tubular heat exchanger, and the second grade heat exchanger is floating head heat exchanger, and wherein, around tubular heat exchanger advantage in heat exchange efficiency is high, and the shortcoming is very easily blockked up, and in case tubular heat exchanger takes place to block up then hardly clears away and leads to, can only change. When silicon powder, hydrogen and silicon tetrachloride are in a fluidized reaction stage in a fluidized bed, a large amount of fine silicon powder is carried by mixed gas to enter the two-stage heat exchanger, so that the risk of tube bundle blockage in the two-stage heat exchanger exists. If the amount of the fine silicon powder brought out from the fluidized bed is too large, the load of the two-stage cyclone separator is further increased, so that the solid content entering a rear-end washing tower is increased, and the quality of the chlorosilane product liquid is seriously influenced.
In the prior art CN106629740A, it is disclosed that hydrogen and hydrogen chloride gas are introduced into a fluidized bed through an electric heater, and the tail gas from a cold hydrogenation reactor is reintroduced into the front-end process for heat exchange, so as to improve the heat utilization rate, save energy, reduce cost, etc.
CN106276918A discloses "an electric heater for heating a mixed gas of silicon tetrachloride and hydrogen and a hydrogenation apparatus for chemically reacting the mixed gas, the hydrogenation apparatus includes multiple hydrogenation reactors connected in series, the mixed gas is heated and then sequentially sent to each hydrogenation reactor to undergo a cold hydrogenation reaction and finally produce a total reaction product gas, which is characterized in that: the system also comprises a device for respectively supplementing hydrogen chloride gas into each stage of hydrogenation reactor. ", wherein the addition of hydrogen chloride, increases the conversion rate.
Disclosure of Invention
In order to solve the defects of the prior art, a trichlorosilane cold hydrogenation production system is provided. In the technical scheme, high-purity hydrogen chloride (more than 99%) is added, and the temperature in the fluidized bed is increased by the exothermic reaction caused by the high-purity hydrogen chloride, so that the reaction quality is improved; and the unreacted silicon powder is consumed, so that the efficiency of subsequent compression and separation is ensured.
In order to achieve the technical purpose, the following technical scheme is proposed:
a trichlorosilane cold hydrogenation production system comprises an electric heater, a fluidized bed reactor, a first-stage heat exchanger, a second-stage heat exchanger and a separator, wherein a discharge port on the electric heater is connected with a feed port on the fluidized bed reactor through a mixed gas pipe, a mixed gas outlet on the fluidized bed reactor is connected with the first-stage heat exchanger through a mixed gas pipe, the first-stage heat exchanger is connected with the second-stage heat exchanger, the second-stage heat exchanger is connected with the separator through a conveying pipe, the separator is connected with a washing tower, and a continuous passage for synthesizing and purifying trichlorosilane is formed among the electric heater, the fluidized bed reactor, the first-stage heat exchanger, the second-stage heat exchanger, the separator and the washing tower;
the mixed gas pipe is connected with a high-purity hydrogen chloride inlet pipe I, one end of the high-purity hydrogen chloride inlet pipe I is communicated with the mixed gas pipe, the other end of the high-purity hydrogen chloride inlet pipe I is connected with a compressor, and the compressor is connected with a high-purity hydrogen chloride source tank;
the mixed gas pipe is connected with a high-purity hydrogen chloride gas inlet pipe II, one end of the high-purity hydrogen chloride gas inlet pipe II is communicated with the mixed gas pipe, and the other end of the high-purity hydrogen chloride gas inlet pipe II is connected with a high-purity hydrogen chloride gas source tank;
and a high-purity hydrogen chloride gas inlet pipe III is connected to the conveying pipe, one end of the high-purity hydrogen chloride gas inlet pipe III is communicated with the conveying pipe, and the other end of the high-purity hydrogen chloride gas inlet pipe III is connected with a high-purity hydrogen chloride gas source tank.
Preferably, the fluidized bed reactor is connected with a silicon powder feeding tank, the electric heater is connected with a silicon tetrachloride/hydrogen vaporizer, the arrangement ensures that each device has definite division of work, and further stably provides a silicon powder raw material and a silicon tetrachloride-hydrogen mixed gas raw material for the fluidized bed reactor, and ensures the orderliness and stability of a trichlorosilane cold hydrogenation production system.
Preferably, the number of the compressors is at least two, and the compressors are arranged in parallel.
Preferably, the high-purity hydrogen chloride inlet pipe I is a high-purity hydrogen chloride inlet pipe I made of 316L materials, the high-purity hydrogen chloride inlet pipe II is a high-purity hydrogen chloride inlet pipe II made of 316L materials, and the high-purity hydrogen chloride inlet pipe III is a high-purity hydrogen chloride inlet pipe III made of 316L materials.
Preferably, the high-purity hydrogen chloride gas source tank is arranged in a reduction section in a polycrystalline silicon production line.
Preferably, the separator is a cyclone separator.
Preferably, the number of the separators is two, and the separators are arranged in series.
Preferably, the slag outlet of the separator is connected with a waste contact tank for collecting waste slag formed in the separation process, so that the sustainability of the production process is ensured; the waste contact tank is connected with the fluidized bed reactor, so that unreacted silicon powder in the fluidized bed reactor is collected, and the influence of residual silicon powder on a cold hydrogenation process is reduced.
Preferably, the liquid outlet of the washing tower is connected with a slurry collecting tank, and slurry formed in the washing procedure is collected, so that the sustainability of the production process is ensured.
In this embodiment, the reaction formula includes:
Si+3HCL→SiHCl 3 +H 2 +Q
in the technical scheme, according to actual requirements, a temperature transmitter, a pressure transmitter, a flowmeter, a valve and the like are arranged on each pipeline.
The positional relationships such as "up", "between", "one end" and "the other end" in the present technical solution are defined according to the actual usage state, and are conventional terms in the technical field and also conventional terms in the actual usage process of the person skilled in the art.
By adopting the technical scheme, the beneficial technical effects brought are as follows:
1. the utility model discloses utilize high-purity HCL gas to get into fluidized bed reactor and silica flour to produce exothermic reaction, promote the fluidized bed reactor internal temperature, reduce electric heater service power, and then reach and reduce the power consumption purpose. In addition, the high-purity HCL gas can supplement chloride ions for the trichlorosilane synthesis reaction, namely the consumption of the raw material silicon tetrachloride is effectively reduced;
2. the utility model discloses in, utilize the reaction of the fine silica flour that high-purity HCL gas and first order heat exchanger import section, second level heat exchanger export section carried, reach and consume fine silica flour, and then can avoid the risk that the tube bundle stopped up in this two-stage heat exchanger to and, separator and scrubbing tower load purpose in the reduction epilogue in addition effectively.
Drawings
Fig. 1 is a flow chart related to the present invention;
in the figure, the device comprises a washing tower 1, a washing tower 2, an electric heater 3, a fluidized bed reactor 4, a first-stage heat exchanger 5, a second-stage heat exchanger 6, a separator 7, a mixed gas pipe 8, high-purity hydrogen chloride gas inlet pipes I and 9, a compressor 10, a high-purity hydrogen chloride gas source tank 11, a mixed gas pipe 12, high-purity hydrogen chloride gas inlet pipes II and 13, a conveying pipe 14, high-purity hydrogen chloride gas inlet pipes III and 15, a silicon powder feeding tank, a silicon tetrachloride/hydrogen vaporizer 16, a waste contact tank 17, a waste contact tank 18 and a slag slurry collecting tank.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
Example 1
A trichlorosilane cold hydrogenation production system comprises an electric heater 2, a fluidized bed reactor 3, a first-stage heat exchanger 4, a second-stage heat exchanger 5 and a separator 6, wherein a discharge port on the electric heater 2 is connected with a feed port on the fluidized bed reactor 3 through a mixed gas pipe 7, a mixed gas outlet on the fluidized bed reactor 3 is connected with the first-stage heat exchanger 4 through a mixed gas pipe 11, the first-stage heat exchanger 4 is connected with the second-stage heat exchanger 5, the second-stage heat exchanger 5 is connected with the separator 6 through a conveying pipe 13, the separator 6 is connected with a washing tower 1, and a continuous passage for synthesizing and purifying trichlorosilane is formed among the electric heater 2, the fluidized bed reactor 3, the first-stage heat exchanger 4, the second-stage heat exchanger 5, the separator 6 and the washing tower 1;
the mixed gas pipe 7 is connected with a high-purity hydrogen chloride inlet pipe I8, one end of the high-purity hydrogen chloride inlet pipe I8 is communicated with the mixed gas pipe 7, the other end of the high-purity hydrogen chloride inlet pipe I8 is connected with a compressor 9, and the compressor 9 is connected with a high-purity hydrogen chloride source tank 10; a high-purity hydrogen chloride inlet pipe II 12 is connected to the mixed gas pipe 11, one end of the high-purity hydrogen chloride inlet pipe II 12 is communicated with the mixed gas pipe 11, and the other end of the high-purity hydrogen chloride inlet pipe II 12 is connected with a high-purity hydrogen chloride source tank 10; the delivery pipe 13 is connected with a high-purity hydrogen chloride inlet pipe III 14, one end of the high-purity hydrogen chloride inlet pipe III 14 is communicated with the delivery pipe 13, and the other end of the high-purity hydrogen chloride inlet pipe III 14 is connected with the high-purity hydrogen chloride source tank 10.
The fluidized bed reactor 3 is connected with a silicon powder feeding tank 15, the electric heater 2 is connected with a silicon tetrachloride/hydrogen vaporizer 16, the arrangement ensures that each device has definite division of work, and further stably provides a mixed gas raw material of silicon powder raw materials and silicon tetrachloride-hydrogen for the fluidized bed reactor 3, and the orderliness and the stability of a trichlorosilane cold hydrogenation production system are ensured.
In the prior art, the reaction temperature in the fluidized bed reactor 3 is maintained by mainly heating and maintaining the electric heater 2, the feeding amount of silicon tetrachloride is maintained at 110t/h, the design power of a single set of the electric heater 2 is 3750KW, the actual opening is 55-70%, the theoretical power is 1875-2625KW, the actual operating power is 2000KW, and under the premise of not considering the shutdown maintenance condition, the reaction temperature is 30X 24X 2000X 0.4= 576000X, and the reaction temperature is 24X 2000X 0.4X 24X 0.4X. If the five systems are operated at full load at the same time, the monthly electricity charge is about 288 ten thousand yuan, and the electricity consumption cost is overhigh.
By adopting the technical scheme, high-purity hydrogen chloride is introduced between the outlet of the electric heater 2 and the inlet section of the fluidized bed reactor 3, the initial setting flow is set to be 300Nm < 3 >/h, the high-purity hydrogen chloride gas enters the fluidized bed reactor 3 to generate exothermic reaction with silicon powder, and the temperature of the fluidized bed reactor 3 is increased through the heat generated by the exothermic reaction, so that the electric heating function is reduced (55-70 percent is reduced to 50-65 percent), and the aim of reducing the power consumption is fulfilled; on the other hand, the reduction byproduct HCl can supplement chloride ions for the trichlorosilane synthesis reaction, and the consumption of the raw material silicon tetrachloride is reduced, namely, high-purity hydrogen chloride is respectively introduced into the inlet section of the first-stage heat exchanger 4 and the outlet section of the second-stage heat exchanger 5 and reacts with the fine silicon powder in the mixed gas to generate trichlorosilane gas through an exothermic reaction, and the reaction is violent and is not easy to control, so that the leakage risk of the heat exchangers is caused, and therefore, the initial flow rates of the two high-purity hydrogen chlorides are set to be 20Nm & lt 3 & gt/h during process control.
Example 2
Based on example 1, this example further limits the introduction of high purity hydrogen chloride to further illustrate the present disclosure.
At least two compressors 9 are arranged, and the compressors 9 are arranged in parallel.
The high-purity hydrogen chloride inlet pipe I8 that relates to is the high-purity hydrogen chloride inlet pipe I8 of 316L material, and high-purity hydrogen chloride advances pipe II to be the high-purity hydrogen chloride inlet pipe II 12 of 316L material, and high-purity hydrogen chloride advances pipe III to be the high-purity hydrogen chloride inlet pipe III 14 of 316L material.
Wherein, the high-purity hydrogen chloride gas source tank 10 is arranged at a reduction working section in the polysilicon production line.
Example 3
Based on the embodiments 1-2, the present embodiment further defines the separator 6 to further describe the technical solution.
The separator 6 is a cyclone separator 6.
The number of the separators 6 is two, and the separators 6 are arranged in series.
A waste contact tank 17 is connected with a slag outlet of the separator 6, and waste slag formed in the separation process is collected, so that the sustainability of the production process is ensured; the waste contact tank 17 is connected with the fluidized bed reactor 3, so that unreacted silicon powder in the fluidized bed reactor 3 is collected, and the influence of residual silicon powder on the cold hydrogenation process is reduced.
Example 4
Based on examples 1-3, this example further defines scrubber 1 to further illustrate the present disclosure.
The liquid outlet of the washing tower 1 is connected with a slurry collecting tank 18 for collecting the slurry formed in the washing procedure, thereby ensuring the sustainability of the production process.
Claims (9)
1. A trichlorosilane cold hydrogenation production system is characterized in that: the device comprises an electric heater (2), a fluidized bed reactor (3), a first-stage heat exchanger (4), a second-stage heat exchanger (5) and a separator (6), wherein a feed port of the electric heater (2) is connected with a feed port of the fluidized bed reactor (3) through a mixed gas pipe (7), a mixed gas outlet of the fluidized bed reactor (3) is connected with the first-stage heat exchanger (4) through a mixed gas pipe (11), the first-stage heat exchanger (4) is connected with the second-stage heat exchanger (5), the second-stage heat exchanger (5) is connected with the separator (6) through a conveying pipe (13), the separator (6) is connected with a washing tower (1), and a continuous passage for synthesizing and purifying trichlorosilane is formed among the electric heater (2), the fluidized bed reactor (3), the first-stage heat exchanger (4), the second-stage heat exchanger (5), the separator (6) and the washing tower (1);
the mixed gas pipe (7) is connected with a high-purity hydrogen chloride inlet pipe I (8), one end of the high-purity hydrogen chloride inlet pipe I (8) is communicated with the mixed gas pipe (7), the other end of the high-purity hydrogen chloride inlet pipe I (8) is connected with a compressor (9), and the compressor (9) is connected with a high-purity hydrogen chloride source tank (10);
a high-purity hydrogen chloride gas inlet pipe II (12) is connected to the mixed gas pipe (11), one end of the high-purity hydrogen chloride gas inlet pipe II (12) is communicated with the mixed gas pipe (11), and the other end of the high-purity hydrogen chloride gas inlet pipe II (12) is connected with a high-purity hydrogen chloride gas source tank (10);
and a high-purity hydrogen chloride inlet pipe III (14) is connected to the conveying pipe (13), one end of the high-purity hydrogen chloride inlet pipe III (14) is communicated with the conveying pipe (13), and the other end of the high-purity hydrogen chloride inlet pipe III (14) is connected with a high-purity hydrogen chloride source tank (10).
2. The trichlorosilane cold hydrogenation production system according to claim 1, wherein the trichlorosilane cold hydrogenation production system comprises: the fluidized bed reactor (3) is connected with a silicon powder feeding tank (15), and the electric heater (2) is connected with a silicon tetrachloride/hydrogen vaporizer (16).
3. The trichlorosilane cold hydrogenation production system according to claim 1, which is characterized in that: the number of the compressors (9) is at least two, and the compressors (9) are arranged in parallel.
4. The trichlorosilane cold hydrogenation production system according to claim 1, which is characterized in that: the high-purity hydrogen chloride inlet pipe I (8) is a high-purity hydrogen chloride inlet pipe I (8) made of 316L materials, the high-purity hydrogen chloride inlet pipe II is a high-purity hydrogen chloride inlet pipe II (12) made of 316L materials, and the high-purity hydrogen chloride inlet pipe III is a high-purity hydrogen chloride inlet pipe III (14) made of 316L materials.
5. The trichlorosilane cold hydrogenation production system according to claim 1, which is characterized in that: the high-purity hydrogen chloride source tank (10) is arranged at a reduction working section in the polycrystalline silicon production line.
6. The trichlorosilane cold hydrogenation production system according to claim 1, which is characterized in that: the separator (6) is a cyclone separator (6).
7. The trichlorosilane cold hydrogenation production system according to claim 1 or 6, wherein: the number of the separators (6) is two, and the separators (6) are arranged in series.
8. The trichlorosilane cold hydrogenation production system according to claim 7, wherein: the slag outlet of the separator (6) is connected with a waste contact tank (17), and the waste contact tank (17) is connected with the fluidized bed reactor (3).
9. The trichlorosilane cold hydrogenation production system according to claim 1, which is characterized in that: and a liquid outlet of the washing tower (1) is connected with a slurry collecting tank (18).
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| Application Number | Priority Date | Filing Date | Title |
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| CN202221949434.2U CN217895154U (en) | 2022-07-27 | 2022-07-27 | Trichlorosilane cold hydrogenation production system |
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| CN202221949434.2U CN217895154U (en) | 2022-07-27 | 2022-07-27 | Trichlorosilane cold hydrogenation production system |
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| CN202221949434.2U Active CN217895154U (en) | 2022-07-27 | 2022-07-27 | Trichlorosilane cold hydrogenation production system |
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