CN104003400A - System for treating polycrystalline silicon tail gas dry-process recovered materials - Google Patents
System for treating polycrystalline silicon tail gas dry-process recovered materials Download PDFInfo
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- CN104003400A CN104003400A CN201410217169.2A CN201410217169A CN104003400A CN 104003400 A CN104003400 A CN 104003400A CN 201410217169 A CN201410217169 A CN 201410217169A CN 104003400 A CN104003400 A CN 104003400A
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Abstract
The invention discloses a system for treating polycrystalline silicon tail gas dry-process recovered materials. The system comprises a first heating device suitable for performing first heating treatment on the recovered materials, a second heating unit which is connected with the first heating device and is suitable for performing second heating treatment on the recovered materials subjected to the first heating treatment, a first rectifying unit which is connected with the second heating unit and is suitable for performing first rectifying treatment on the recovered materials subjected to the second heating treatment to obtain first tower top vapor and first tower bottom liquid and returning the first tower bottom liquid serving as a heat source to the second heating unit, and a second rectifying device which is connected with the first rectifying unit and is suitable for performing second rectifying treatment on the first tower top vapor to obtain a liquid-state light component and second tower bottom liquid and returning the second tower bottom liquid serving as a heat source to the first heating device. According to the system, heat energy and cold energy can be optimally and comprehensively utilized, so that the equipment investment and the energy consumption are remarkably reduced.
Description
Technical field
The invention belongs to field of polysilicon production, particularly, the present invention relates to a kind of system of processing polycrystalline silicon tail gas dry reclaimed materials.
Background technology
Polysilicon is the crucial starting material of unicircuit and photovoltaic generation, and dry back rewinding is as the intermediates in production of polysilicon technique, and the quality of its processing directly affects quality and the energy consumption of unit product of polysilicon product.At present, along with the continuous expansion of production of polysilicon scale, need dry back rewinding amount to be processed to increase gradually, and at present common way is for copying and increasing production line, has so significantly increased energy consumption and the facility investment of processing dry back rewinding.
Thereby the technology of existing processing polycrystalline silicon tail gas dry reclaimed materials is further improved.
Summary of the invention
The present invention one of is intended to solve the problems of the technologies described above at least to a certain extent or at least provides a kind of useful business to select.For this reason, one object of the present invention is to propose a kind of system of processing polycrystalline silicon tail gas dry reclaimed materials, and this system can realize the optimal synthesis utilization of heat and cold, thereby significantly reduces facility investment and energy consumption.
In one aspect of the invention, the present invention proposes a kind of system of processing polycrystalline silicon tail gas dry reclaimed materials, described reclaimed materials contains dichloro-dihydro silicon, trichlorosilane and silicon tetrachloride, and this system comprises:
First heater, described first heater is suitable for described reclaimed materials to carry out the first heat treated, to obtain the reclaimed materials through the first heat treated;
The second heating unit, described the second heating unit is connected with described first heater, and is suitable for the described reclaimed materials through the first heat treated to carry out the second heat treated, to obtain the reclaimed materials through the second heat treated;
The first rectification cell, described the first rectification cell is connected with described the second heating unit, and be suitable for the described reclaimed materials through the second heat treated to carry out the first rectification process, to obtain the first overhead vapours and the first tower bottoms, described the first tower bottoms contains silicon tetrachloride, and using described the first tower bottoms as thermal source, be back to described the second heating unit, to obtain silicon tetrachloride; And
The second rectifier unit, described the second rectifier unit is connected with described the first rectification cell, and be suitable for described the first overhead vapours to carry out the second rectification process, to obtain liquid light constituent and the second tower bottoms, described the second tower bottoms contains trichlorosilane, and described the second tower bottoms is back to described first heater as thermal source, to obtain trichlorosilane.
According to the system of the processing polycrystalline silicon tail gas dry reclaimed materials of the embodiment of the present invention, by treating rectifying material using the resulting tower bottoms of rectification process process as thermal source, carry out thermal pretreatment, make tower bottoms be lowered the temperature simultaneously, and then realized the comprehensive utilization of heat and cold, thereby facility investment and energy consumption have significantly been reduced.
In addition, the system of processing polycrystalline silicon tail gas dry reclaimed materials according to the above embodiment of the present invention can also have following additional technical characterictic:
In some embodiments of the invention, the system of described processing polycrystalline silicon tail gas dry reclaimed materials further comprises: surge tank, described surge tank is connected with described the second rectifier unit with described the first rectification cell, and before being suitable for being stored in and carrying out described the second rectification process, thermal source using described the first overhead vapours as described the second rectifier unit and the overhead vapours phlegma that obtains, and a part for described overhead vapours phlegma is back to described the first rectification cell, and another part of described overhead vapours phlegma is passed into described the second rectifier unit.Thus, can realize the comprehensive utilization of heat and cold.
In some embodiments of the invention, described the second heating unit further comprises: the 3rd heating unit, described the 3rd heating unit is connected with described first heater, and be suitable for the described reclaimed materials through the first heat treated to carry out the 3rd heat treated, to obtain the reclaimed materials through the 3rd heat treated; And the 4th heating unit, described the 4th heating unit is connected with described the 3rd heating unit, and is suitable for the described reclaimed materials through the 3rd heat treated to carry out the 4th heat treated, to obtain the described reclaimed materials through the second heat treated.Thus, can significantly improve the pre-thermo-efficiency of material.
In some embodiments of the invention, described the first rectification cell further comprises: the 3rd rectifier unit, described the 3rd rectifier unit is connected with described the 4th heating unit, and be suitable for a part for the described reclaimed materials through the second heat treated to carry out the 3rd rectification process, to obtain the 3rd overhead vapours and the 3rd tower bottoms; And the 4th rectifier unit, described the 4th rectifier unit is connected with described the 4th heating unit, and is suitable for another part of the described reclaimed materials through the second heat treated to carry out the 4th rectification process, to obtain the 4th overhead vapours and the 4th tower bottoms.Thus, can significantly improve the rectification efficiency of material.
In some embodiments of the invention, the system of described processing polycrystalline silicon tail gas dry reclaimed materials further comprises: the first refrigerating unit, described the first refrigerating unit is connected with described the second rectifier unit, and be suitable for described liquid light constituent to carry out the first cooling process, so that separation obtains dichloro-dihydro silicon.Thus, can separation obtain dichloro-dihydro silicon.
In some embodiments of the invention, described surge tank is connected with described the second rectifier unit with described the 3rd rectifier unit, described the 4th rectifier unit respectively, and be suitable for the first part of described overhead vapours phlegma to be back to described the 3rd rectifier unit, the second section of described overhead vapours phlegma is back to described the 4th rectifier unit, the third part of described overhead vapours phlegma is passed into described the second rectifier unit.Thus, can realize the utilization ratio of material.
In some embodiments of the invention, described the 3rd rectifier unit is connected with the shell side opening for feed on described the 4th heating unit respectively with described the 4th rectifier unit, and be suitable for described the 3rd tower bottoms and described the 4th tower bottoms one of at least as thermal source, to be back to described the 4th heating unit, to obtain the silicon tetrachloride of the first cooling, shell side discharge port on described the 4th heating unit is connected with the shell side opening for feed on described the 3rd heating unit, and be suitable for the silicon tetrachloride of described the first cooling to be back to described the 3rd heating unit as thermal source, to obtain the silicon tetrachloride of the second cooling.Thus, can further realize the optimal synthesis utilization of system thermal and cold.
In some embodiments of the invention, the system of described processing polycrystalline silicon tail gas dry reclaimed materials further comprises: the second refrigerating unit, described the second refrigerating unit is connected with described the 3rd heating unit, and be suitable for the silicon tetrachloride of described the second cooling to carry out the second cooling process, to obtain described silicon tetrachloride.Thus, can separation obtain silicon tetrachloride.
In some embodiments of the invention, described the second rectifier unit is connected with described first heater, and is suitable for described the second tower bottoms to be back to described first heater as thermal source, to obtain the second tower bottoms of cooling.Thus, can further improve the optimal synthesis utilization of system thermal and cold.
In some embodiments of the invention, the system of described processing polycrystalline silicon tail gas dry reclaimed materials further comprises: the 3rd refrigerating unit, described the 3rd refrigerating unit is connected with described the second rectifier unit, and be suitable for the second tower bottoms of described cooling to carry out the 3rd cooling process, to obtain trichlorosilane.Thus, can separation obtain trichlorosilane.
Additional aspect of the present invention and advantage in the following description part provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage accompanying drawing below combination obviously and is easily understood becoming the description of embodiment, wherein:
Fig. 1 is the structural representation of processing according to an embodiment of the invention the system of polycrystalline silicon tail gas dry reclaimed materials;
Fig. 2 is the structural representation of system of the processing polycrystalline silicon tail gas dry reclaimed materials of another embodiment according to the present invention;
Fig. 3 utilizes the system implementation of the processing polycrystalline silicon tail gas dry reclaimed materials of one embodiment of the invention to process the schematic flow sheet of the method for polycrystalline silicon tail gas dry reclaimed materials;
Fig. 4 utilizes the system implementation of the processing polycrystalline silicon tail gas dry reclaimed materials of another embodiment of the present invention to process the schematic flow sheet of the method for polycrystalline silicon tail gas dry reclaimed materials;
Fig. 5 is the structural representation of system of the processing polycrystalline silicon tail gas dry reclaimed materials of another embodiment according to the present invention.
Embodiment
Describe embodiments of the invention below in detail, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has the element of identical or similar functions from start to finish.Below by the embodiment being described with reference to the drawings, be exemplary, be intended to for explaining the present invention, and can not be interpreted as limitation of the present invention.
In description of the invention, it will be appreciated that, term " " center ", " longitudinally ", " laterally ", " length ", " width ", " thickness ", " on ", D score, " front ", " afterwards ", " left side ", " right side ", " vertically ", " level ", " top ", " end " " interior ", " outward ", " clockwise ", orientation or the position relationship of indications such as " counterclockwise " are based on orientation shown in the drawings or position relationship, only the present invention for convenience of description and simplified characterization, rather than device or the element of indication or hint indication must have specific orientation, with specific orientation structure and operation, therefore can not be interpreted as limitation of the present invention.
In addition, term " first ", " second " be only for describing object, and can not be interpreted as indication or hint relative importance or the implicit quantity that indicates indicated technical characterictic.Thus, one or more these features can be expressed or impliedly be comprised to the feature that is limited with " first ", " second ".In description of the invention, the implication of " a plurality of " is two or more, unless otherwise expressly limited specifically.
In the present invention, unless otherwise clearly defined and limited, the terms such as term " installation ", " being connected ", " connection ", " fixing " should be interpreted broadly, and for example, can be to be fixedly connected with, and can be also to removably connect, or connect integratedly; Can be mechanical connection, can be to be also electrically connected to; Can be to be directly connected, also can indirectly be connected by intermediary, can be the connection of two element internals.For the ordinary skill in the art, can understand as the case may be above-mentioned term concrete meaning in the present invention.
In the present invention, unless otherwise clearly defined and limited, First Characteristic Second Characteristic it " on " or D score can comprise that the first and second features directly contact, also can comprise that the first and second features are not directly contacts but contact by the other feature between them.And, First Characteristic Second Characteristic " on ", " top " and " above " comprise First Characteristic directly over Second Characteristic and oblique upper, or only represent that First Characteristic level height is higher than Second Characteristic.First Characteristic Second Characteristic " under ", " below " and " below " comprise First Characteristic under Second Characteristic and tiltedly, or only represent that First Characteristic level height is less than Second Characteristic.
In one aspect of the invention, the present invention proposes a kind of system of processing polycrystalline silicon tail gas dry reclaimed materials.Below with reference to Fig. 1-2, the system of the processing polycrystalline silicon tail gas dry reclaimed materials of the embodiment of the present invention is described in detail.According to embodiments of the invention, this system comprises:
First heater 100: according to embodiments of the invention, first heater 100 is suitable for reclaimed materials to carry out the first heat treated, thereby can obtain the reclaimed materials through the first heat treated.If no special instructions, the reclaimed materials of mentioning is herein in polysilicon production process and adopts " improved Siemens " to reclaim the reclaimed materials that polysilicon tail gas obtains.According to embodiments of the invention, reclaimed materials can contain dichloro-dihydro silicon, trichlorosilane and silicon tetrachloride.According to embodiments of the invention, the condition of the first heat treated is also not particularly limited, and according to a particular embodiment of the invention, the first heat treated can be carried out at the temperature of 25～40 degrees Celsius.Particularly, first heater can be interchanger, for example, can be vertical two-tube-pass monoshell pass heat exchanger.
The second heating unit 200: according to embodiments of the invention, the second heating unit 200 is connected with first heater 100, and be suitable for the reclaimed materials through the first heat treated obtained above to carry out the second heat treated, thereby can obtain the reclaimed materials through the second heat treated.According to embodiments of the invention, the second heating unit can comprise a plurality of heating units, for example can comprise the 3rd heating unit and two devices of the 4th heating unit, concrete, the 3rd heating unit is connected with first heater, be suitable for the reclaimed materials through the first heat treated to carry out the 3rd heat treated in the 3rd heating unit, thereby can obtain the reclaimed materials through the 3rd heat treated, the 4th heating unit is connected with the 3rd heating unit, be suitable for the resulting reclaimed materials through the 3rd heat treated to carry out the 4th heat treated in the 4th heating unit, thereby can obtain the reclaimed materials through the second heat treated.According to embodiments of the invention, the condition of the 3rd heat treated and the 4th heat treated is also not particularly limited, according to a particular embodiment of the invention, the 3rd heat treated can be carried out under the pressure of the temperature of 40～55 degrees Celsius and 0.4～0.6MPa, and the 4th heat treated can be carried out under the pressure of the temperature of 55～70 degrees Celsius and 0.4～0.6MPa.Particularly, the 3rd heating unit and the 4th heating unit can be all interchanger, for example, can be vertical two-tube-pass monoshell pass heat exchanger.
The first rectification cell 300: according to embodiments of the invention, the first rectification cell 300 is connected with the second heating unit 200, and be suitable for through the second heat treated reclaimed materials, carrying out the first rectification process by obtained above, thereby can obtain the first overhead vapours and the first tower bottoms, according to a particular embodiment of the invention, the first tower bottoms contains silicon tetrachloride.According to embodiments of the invention, the first rectification cell can comprise a plurality of rectifier units, for example can comprise two of the 3rd rectifier unit and the 4th rectifier units, particularly, the 3rd rectifier unit is connected with the 4th heating unit, be suitable for a part for the reclaimed materials through the second heat treated obtained above being carried out in the 3rd rectifier unit to the 3rd rectification process, thereby can obtain the 3rd overhead vapours and the 3rd tower bottoms.Meanwhile, the 4th rectifier unit is connected with the 4th heating unit, is suitable for another part of the above-mentioned resulting reclaimed materials through the second heat treated being carried out in the 4th rectifier unit to the 4th rectification process, thereby can obtains the 4th overhead vapours and the 4th tower bottoms.It should be noted that, the 3rd overhead vapours and the 4th overhead vapours are converged and be the first overhead vapours, the 3rd tower bottoms and the 4th tower bottoms are converged and be the first tower bottoms.According to embodiments of the invention, the condition of the 3rd rectification process and the 4th rectification process is also not particularly limited, according to a particular embodiment of the invention, the 3rd rectification process and the 4th rectification process all can be carried out under the pressure of the temperature of 80～120 degrees Celsius and 0.3～0.5MPa.Contriver finds, under this condition, can obviously improve rectification process efficiency.According to embodiments of the invention, the temperature of the first tower bottoms can be 110～130 degrees Celsius, and the temperature of the first overhead vapours can be 75～95 degrees Celsius.According to embodiments of the invention, the 3rd rectifier unit and the 4th rectifier unit all can adopt regular packed tower or tray column, the scope of theoretical plate number is 60～80, the scope of tower top operation table pressure is 0.35～0.55MPa, the scope of tower top service temperature is 80～95 ℃, and quantity of reflux is 2～6 with the scope of the mass flow rate ratio of inlet amount.
According to embodiments of the invention, using the first tower bottoms obtaining in the first rectification cell as thermal source, be back to the second heating unit and carry out the second heat treated, thereby can obtain silicon tetrachloride.As mentioned above, secondary heating mechanism can comprise the 3rd heating unit and the 4th heating unit.According to embodiments of the invention, the 3rd heating unit and the 4th heating unit can be all vertical two-tube-pass monoshell pass heat exchanger, wherein high-temperature material is walked shell side, low-temperature material is walked tube side, by two-direction heat-exchanging, processes, and can realize the cooling of high-temperature material and the preheating of low-temperature material simultaneously.Particularly, first above resulting the 3rd tower bottoms and the 4th tower bottoms one of at least carried out to the 4th heat treated in the 4th heating unit as thermal source, wherein, the 3rd tower bottoms and the 4th tower bottoms enter shell side from shell side upper orifice, from shell side lower nozzle, discharge, reclaimed materials through the 3rd heat treated is walked tube side, and the shell side top charging mouth of pipe and the tube side discharging mouth of pipe are in same orientation, through two-direction heat-exchanging, process, the heat of the 3rd tower bottoms and the 4th tower bottoms is absorbed by the reclaimed materials through the 3rd heat treated, thereby can obtain the reclaimed materials through the second heat treated of 65～75 degrees Celsius and the first cooling silicon tetrachloride of 75～95 degrees Celsius, then, the silicon tetrachloride of resulting the first cooling is carried out to the 3rd heat treated in the 3rd rectifier unit as thermal source, wherein, the silicon tetrachloride of the first cooling enters shell side from shell side upper orifice, from shell side lower nozzle, discharge, reclaimed materials through the first heat treated is walked tube side, and the shell side top charging mouth of pipe and the tube side discharging mouth of pipe are in same orientation, through two-direction heat-exchanging, process, the heat of the silicon tetrachloride of the first cooling is absorbed by the reclaimed materials through the first heat treated, thereby can obtain the reclaimed materials through the 3rd heat treated of 45～65 degrees Celsius and the second cooling silicon tetrachloride of 40～60 degrees Celsius, finally the silicon tetrachloride of resulting the second cooling is carried out to the second cooling process in the second refrigerating unit, thereby can obtain silicon tetrachloride product.According to embodiments of the invention, can adopt water-cooling pattern to carry out the second cooling process to the silicon tetrachloride of the second cooling.According to embodiments of the invention, the condition of the second cooling process is also not particularly limited, and according to a particular embodiment of the invention, the second cooling process can be carried out under the pressure of the temperature of 25～55 degrees Celsius and 0.3～0.5MPa.Contriver finds in surprise through great many of experiments, through the resulting tower bottoms of the first rectification process, can carry out thermal pretreatment for the reclaimed materials to through the first heat treated, and by the heat of tower bottoms is used for the reclaimed materials through the first heat treated to carry out heat treated, can significantly improve the temperature of reclaimed materials and the temperature of reduction tower bottoms through the first heat treated, thereby can fully realize the comprehensive utilization of heat and cold, and then reduce investment and the energy consumption of equipment.
The second rectifier unit 400: according to embodiments of the invention, the second rectifier unit 400 is connected with the first rectification cell 300, and be suitable for the first overhead vapours obtained above to carry out the second rectification process, thereby can obtain liquid light constituent and the second tower bottoms, according to a particular embodiment of the invention, in liquid light constituent, contain in dichloro-dihydro silicon, the second tower bottoms and contain trichlorosilane.According to embodiments of the invention, the condition of the second rectification process is also not particularly limited, and according to a particular embodiment of the invention, the second rectification process can be carried out under the pressure of the temperature of 45～75 degrees Celsius and 0.2～0.4MPa.Contriver finds, under this condition, can obviously improve rectification process efficiency.According to embodiments of the invention, the second rectification process can adopt regular packed tower, the scope of theoretical plate number is 100～120, the scope of tower top operation table pressure is 0.2～0.4MPa, the scope of tower top service temperature is 50～65 ℃, and quantity of reflux is 4～8 with the scope of the mass flow rate ratio of inlet amount.
According to embodiments of the invention, can in first heater, carry out using the second tower bottoms as thermal source the first heat treated, thereby can obtain trichlorosilane.According to embodiments of the invention, first heater can adopt vertical two-tube-pass monoshell pass heat exchanger.Concrete, first above-mentioned second tower bottoms that obtains is carried out to the first heat treated in first heater as thermal source, wherein, the second tower bottoms is walked from shell side upper orifice and is entered shell side, from shell side lower nozzle, discharge, reclaimed materials is walked tube side, and the shell side top charging mouth of pipe and the tube side discharging mouth of pipe are in same orientation, through two-direction heat-exchanging, process, the heat of the second tower bottoms is recovered material and absorbs, thereby can obtain the second tower bottoms of the cooling of the reclaimed materials through the first heat treated of 30～50 degrees Celsius and 30～50 degrees Celsius, then the second tower bottoms of resulting cooling is carried out in the 3rd refrigerating unit to the 3rd cooling process, thereby can obtain trichlorosilane.According to embodiments of the invention, the condition of the 3rd cooling process is also not particularly limited, and according to a particular embodiment of the invention, the 3rd cooling process can be carried out under the pressure of the temperature of 20～40 degrees Celsius and 0.2～0.4MPa.Contriver finds, through the second rectification process, obtaining the second tower bottoms can be for carrying out thermal pretreatment to reclaimed materials, and by the heat of tower bottoms is used for reclaimed materials to carry out heat treated, can significantly improve the temperature of reclaimed materials and the temperature of reduction tower bottoms, thereby further fully realize the comprehensive utilization of heat and cold, and then reduce investment and the energy consumption of equipment.
According to the system of the processing polycrystalline silicon tail gas dry reclaimed materials of the embodiment of the present invention, by treating rectifying material using the resulting tower bottoms of rectification process process as thermal source, carry out thermal pretreatment, make tower bottoms be lowered the temperature simultaneously, and then realized the comprehensive utilization of heat and cold, thereby facility investment and energy consumption have significantly been reduced.
With reference to figure 2, the system of the processing polycrystalline silicon tail gas dry reclaimed materials of the embodiment of the present invention further comprises:
Surge tank 500: according to embodiments of the invention, surge tank 500 is connected with the second rectifier unit 400 with the first rectification cell 300 respectively, and before being suitable for being stored in and carrying out the second rectification process, the overhead vapours phlegma obtaining the first overhead vapours as the thermal source of the second rectifier unit, and a part for overhead vapours phlegma is back to the first rectification cell, and another part of overhead vapours phlegma is passed into the second rectifier unit.Particularly, surge tank is connected with the 3rd rectifier unit, the 4th rectifier unit, the second rectifier unit respectively, be suitable for resulting the 3rd overhead vapours and the 4th overhead vapours (the first overhead vapours) as thermal source for the reboiler in the second rectifier unit provides heat, thereby can store tower top steam condensate, and the first part of steam condensate is returned and carries out the 3rd rectifier unit, the second section of steam condensate is returned and carries out the 4th rectifier unit, the third part of overhead vapours phlegma is passed into and in the second rectifier unit, carries out the second rectification process.Contriver finds, resulting the first overhead vapours of the first rectification process process can be used as thermal source provides heat to the second rectification process process, thereby can further take full advantage of the heat producing in system, and then significantly reduce investment and the energy consumption input of equipment.
The first refrigerating unit 600: according to embodiments of the invention, the first refrigerating unit 600 is connected with the second rectifier unit 400, and is suitable for resulting liquid light constituent to carry out the first cooling process, thereby can separation obtain dichloro-dihydro silicon.According to embodiments of the invention, the first cooling process can be carried out under the pressure of the temperature of 20～40 degrees Celsius and 0.2～0.4MPa.According to a particular embodiment of the invention, refrigerating unit can be water cooling plant.
Above the system of the processing polycrystalline silicon tail gas dry reclaimed materials of the embodiment of the present invention be have been described in detail, for convenient, understand, the method for utilizing the system implementation of the processing polycrystalline silicon tail gas dry reclaimed materials of the embodiment of the present invention to process polycrystalline silicon tail gas dry reclaimed materials below with reference to Fig. 3-4 pair is described in detail.According to embodiments of the invention, the method comprises:
S100: the first heat treated
According to embodiments of the invention, reclaimed materials is carried out to the first heat treated, thereby can obtain the reclaimed materials through the first heat treated.As mentioned above, the reclaimed materials of mentioning is herein in polysilicon production process and adopts " improved Siemens " to reclaim the reclaimed materials that polysilicon tail gas obtains.According to embodiments of the invention, reclaimed materials can contain dichloro-dihydro silicon, trichlorosilane and silicon tetrachloride.According to embodiments of the invention, the condition of the first heat treated is also not particularly limited, and according to a particular embodiment of the invention, the first heat treated can be carried out at the temperature of 25～40 degrees Celsius.Particularly, the first heat treated can adopt interchanger to carry out, for example, can adopt vertical two-tube-pass monoshell pass heat exchanger.
S200: the second heat treated
According to embodiments of the invention, the reclaimed materials through the first heat treated obtained above is carried out to the second heat treated, thereby can obtain the reclaimed materials through the second heat treated.According to embodiments of the invention, the second heat treated can comprise multistep heat treated, for example can comprise the 3rd heat treated and the 4th heat treated two steps, concrete, reclaimed materials through the first heat treated is carried out to the 3rd heat treated, thereby can obtain the reclaimed materials through the 3rd heat treated, then the resulting reclaimed materials through the 3rd heat treated be carried out to the 4th heat treated, thereby can obtain the reclaimed materials through the second heat treated.According to embodiments of the invention, the condition of the 3rd heat treated and the 4th heat treated is also not particularly limited, according to a particular embodiment of the invention, the 3rd heat treated can be carried out under the pressure of the temperature of 40～55 degrees Celsius and 0.4～0.6MPa, and the 4th heat treated can be carried out under the pressure of the temperature of 55～70 degrees Celsius and 0.4～0.6MPa.Particularly, the 3rd heat treated and the 4th heat treated all can adopt interchanger to carry out, for example, can adopt vertical two-tube-pass monoshell pass heat exchanger.
S300: the first rectification process
According to embodiments of the invention, by obtained above, through the second heat treated reclaimed materials, carry out the first rectification process, thereby can obtain the first overhead vapours and the first tower bottoms, according to a particular embodiment of the invention, the first tower bottoms contains silicon tetrachloride.According to embodiments of the invention, the first rectification process can comprise multistep rectification process, for example can comprise the 3rd rectification process and the 4th rectification process two steps, particularly, a part for reclaimed materials through the second heat treated obtained above is carried out to the 3rd rectification process, thereby can obtain the 3rd overhead vapours and the 3rd tower bottoms.Meanwhile, another part of the above-mentioned resulting reclaimed materials through the second heat treated is carried out to the 4th rectification process, thereby can obtain the 4th overhead vapours and the 4th tower bottoms.It should be noted that, the 3rd overhead vapours and the 4th overhead vapours are converged and be the first overhead vapours, the 3rd tower bottoms and the 4th tower bottoms are converged and be the first tower bottoms.According to embodiments of the invention, the condition of the 3rd rectification process and the 4th rectification process is also not particularly limited, according to a particular embodiment of the invention, the 3rd rectification process and the 4th rectification process all can be carried out under the pressure of the temperature of 80～120 degrees Celsius and 0.3～0.5MPa.Contriver finds, under this condition, can obviously improve rectification process efficiency.According to embodiments of the invention, the temperature of the first tower bottoms can be 110～130 degrees Celsius, and the temperature of the first overhead vapours can be 75～95 degrees Celsius.According to embodiments of the invention, the 3rd rectification process and the 4th rectification process all can adopt regular packed tower or tray column, the scope of theoretical plate number is 60～80, the scope of tower top operation table pressure is 0.35～0.55MPa, the scope of tower top service temperature is 80～95 ℃, and quantity of reflux is 2～6 with the scope of the mass flow rate ratio of inlet amount.
S400: the second rectification process
According to embodiments of the invention, the first overhead vapours obtained above is carried out to the second rectification process, thereby can obtain liquid light constituent and the second tower bottoms, according to a particular embodiment of the invention, in liquid light constituent, contain in dichloro-dihydro silicon, the second tower bottoms and contain trichlorosilane.According to embodiments of the invention, the condition of the second rectification process is also not particularly limited, and according to a particular embodiment of the invention, the second rectification process can be carried out under the pressure of the temperature of 45～75 degrees Celsius and 0.2～0.4MPa.Contriver finds, under this condition, can obviously improve rectification process efficiency.According to embodiments of the invention, the second rectification process can adopt regular packed tower, the scope of theoretical plate number is 100～120, the scope of tower top operation table pressure is 0.2～0.4MPa, the scope of tower top service temperature is 50～65 ℃, and quantity of reflux is 4～8 with the scope of the mass flow rate ratio of inlet amount.
S500: carry out the second heat treated using the first tower bottoms as thermal source
According to embodiments of the invention, the first tower bottoms that S300 is obtained carries out the second heat treated in S200 as thermal source, thereby can obtain silicon tetrachloride.As mentioned above, the second heat treated can comprise the 3rd heat treated and the 4th heat treated.According to embodiments of the invention, the 3rd heat treated and the 4th heat treated all can adopt vertical two-tube-pass monoshell pass heat exchanger, wherein high-temperature material is walked shell side, low-temperature material is walked tube side, by two-direction heat-exchanging, processes, and can realize the cooling of high-temperature material and the preheating of low-temperature material simultaneously.In this step, particularly, first above resulting the 3rd tower bottoms and the 4th tower bottoms one of at least carried out to the 4th heat treated as thermal source, wherein, the 3rd tower bottoms and the 4th tower bottoms enter shell side from shell side upper orifice, from shell side lower nozzle, discharge, reclaimed materials through the 3rd heat treated is walked tube side, and the shell side top charging mouth of pipe and the tube side discharging mouth of pipe are in same orientation, through two-direction heat-exchanging, process, the heat of the 3rd tower bottoms and the 4th tower bottoms is absorbed by the reclaimed materials through the 3rd heat treated, thereby can obtain the reclaimed materials through the second heat treated of 65～75 degrees Celsius and the first cooling silicon tetrachloride of 75～95 degrees Celsius, then, the silicon tetrachloride of resulting the first cooling is carried out to the 3rd heat treated as thermal source, wherein, the silicon tetrachloride of the first cooling enters shell side from shell side upper orifice, from shell side lower nozzle, discharge, reclaimed materials through the first heat treated is walked tube side, and the shell side top charging mouth of pipe and the tube side discharging mouth of pipe are in same orientation, through two-direction heat-exchanging, process, the heat of the silicon tetrachloride of the first cooling is absorbed by the reclaimed materials through the first heat treated, thereby can obtain the reclaimed materials through the 3rd heat treated of 45～65 degrees Celsius and the second cooling silicon tetrachloride of 40～60 degrees Celsius, finally the silicon tetrachloride of resulting the second cooling is carried out to the second cooling process, thereby can obtain silicon tetrachloride product.According to embodiments of the invention, can adopt water-cooling pattern to carry out the second cooling process to the silicon tetrachloride of the second cooling.According to embodiments of the invention, the condition of the second cooling process is also not particularly limited, and according to a particular embodiment of the invention, the second cooling process can be carried out under the pressure of the temperature of 25～55 degrees Celsius and 0.3～0.5MPa.Contriver finds in surprise through great many of experiments, through the resulting tower bottoms of the first rectification process, can carry out thermal pretreatment for the reclaimed materials to through the first heat treated, and by the heat of tower bottoms is used for the reclaimed materials through the first heat treated to carry out heat treated, can significantly improve the temperature of reclaimed materials and the temperature of reduction tower bottoms through the first heat treated, thereby can fully realize the comprehensive utilization of heat and cold, and then reduce investment and the energy consumption of equipment.
S600: carry out the first heat treated using the second tower bottoms as thermal source
According to embodiments of the invention, the second tower bottoms that S400 is obtained carries out the first heat treated in S100 as thermal source, thereby can obtain trichlorosilane.According to embodiments of the invention, the first heat treated can adopt vertical two-tube-pass monoshell pass heat exchanger.In this step, concrete, first above-mentioned second tower bottoms that obtains is carried out to the first heat treated as thermal source, wherein, the second tower bottoms enters shell side from shell side upper orifice, from shell side lower nozzle, discharge, reclaimed materials is walked tube side, and the shell side top charging mouth of pipe and the tube side discharging mouth of pipe are in same orientation, through two-direction heat-exchanging, process, the heat of the second tower bottoms is recovered material and absorbs, thereby can obtain the second tower bottoms of the cooling of the reclaimed materials through the first heat treated of 30～50 degrees Celsius and 30～50 degrees Celsius, then the second tower bottoms of resulting cooling is carried out to the 3rd cooling process, thereby can obtain trichlorosilane.According to embodiments of the invention, the condition of the 3rd cooling process is also not particularly limited, and according to a particular embodiment of the invention, the 3rd cooling process can be carried out under the pressure of the temperature of 20～40 degrees Celsius and 0.2～0.4MPa.Contriver finds, through the second rectification process, obtaining the second tower bottoms can be for carrying out thermal pretreatment to reclaimed materials, and by the heat of tower bottoms is used for reclaimed materials to carry out heat treated, can significantly improve the temperature of reclaimed materials and the temperature of reduction tower bottoms, thereby further fully realize the comprehensive utilization of heat and cold, and then reduce investment and the energy consumption of equipment.
According to the method for the processing polycrystalline silicon tail gas dry reclaimed materials of the embodiment of the present invention, by treating rectifying material using the resulting tower bottoms of rectification process process as thermal source, carry out thermal pretreatment, make tower bottoms be lowered the temperature simultaneously, and then realized the comprehensive utilization of heat and cold, thereby facility investment and energy consumption have significantly been reduced.
With reference to figure 4, the method for the processing polycrystalline silicon tail gas dry reclaimed materials of the embodiment of the present invention further comprises:
S700: carry out the second rectification process using the first overhead vapours as thermal source
According to embodiments of the invention, at the first overhead vapours that S300 is obtained, carried out before the first rectification process, using the first overhead vapours as thermal source, in S400, carry out the second rectification process, thereby can obtain overhead vapours phlegma, and a part for overhead vapours phlegma is returned and carried out the first rectification process, another part of overhead vapours phlegma is carried out to the second rectification process.In this step, particularly, using resulting the 3rd overhead vapours and the 4th overhead vapours (the first overhead vapours), as thermal source, to the reboiler in the second rectification process process, provide heat, thereby can obtain overhead vapours phlegma, and the first part of steam condensate is returned and carries out the 3rd rectification process, the second section of steam condensate is returned and carries out the 4th rectification process, the third part of overhead vapours phlegma is carried out to the second rectification process.Contriver finds, resulting the first overhead vapours of the first rectification process process can be used as thermal source provides heat to the second rectification process process, thereby can further take full advantage of the heat producing in system, and then significantly reduce investment and the energy consumption input of equipment.
S800: the first cooling process
According to embodiments of the invention, the resulting liquid light constituent of S400 is carried out to the first cooling process, thereby can separation obtain dichloro-dihydro silicon.According to embodiments of the invention, the condition of the first cooling process is also not particularly limited, and according to a particular embodiment of the invention, the first cooling process can be carried out under the pressure of the temperature of 20～40 degrees Celsius and 0.2～0.4MPa.According to a particular embodiment of the invention, cooling process can adopt water cooling plant.
As mentioned above, according to the method for the processing polycrystalline silicon tail gas dry reclaimed materials of the embodiment of the present invention, can have and be selected from following advantage one of at least:
According to the method for the processing polycrystalline silicon tail gas dry reclaimed materials of the embodiment of the present invention, by distillation system, integrate, to a certain degree reduced facility investment and the energy expenditure of system;
The thermal source and the low-temperature receiver that according to the method for the processing polycrystalline silicon tail gas dry reclaimed materials of the embodiment of the present invention, make full use of internal system, reach the optimal synthesis utilization of energy, further reduces energy expenditure and the running cost of system.
Below with reference to specific embodiment, present invention is described, it should be noted that, these embodiment are only descriptive, and do not limit the present invention in any way.
Embodiment
As shown in Figure 5, polycrystalline silicon tail gas dry reclaimed materials is carried out in first heater 100 to the first heat treated, then the resulting reclaimed materials through the first heat treated is carried out to the 3rd heat treated in the 3rd heating unit 210, then the resulting reclaimed materials through the 3rd heat treated is carried out to the 4th heat treated in the 4th heating unit 220, obtain the reclaimed materials through the second heat treated, then the part obtaining through the reclaimed materials of the second heat treated is carried out to the 3rd heat treated in the 3rd rectifier unit 310, obtain the 3rd overhead vapours and the 3rd tower bottoms, another part of the reclaimed materials through the second heat treated obtaining is carried out in the 4th rectifier unit 320 to the 4th rectification process, obtain the 4th overhead vapours and the 4th tower bottoms, then the heat one of at least of the 3rd overhead vapours and the 4th overhead vapours is supplied to the reboiler 410 of the second rectifier unit 400, obtaining steam condensate is stored in surge tank 500, the first part of steam condensate is back to the 3rd rectifier unit, the second section of steam condensate is back to the 4th rectifier unit, the third part of steam condensate is supplied in the second rectifier unit 400 and carries out the second rectification process, obtain liquid light constituent and the second tower bottoms, the heat one of at least of above resulting the 3rd tower bottoms and the 4th tower bottoms is supplied in the 4th heating unit 220 simultaneously, by two-direction heat-exchanging, process, obtain the silicon tetrachloride of the first cooling, then the heat of the silicon tetrachloride of the first cooling obtaining is supplied in the 3rd heating unit 210, obtain the silicon tetrachloride of the second cooling, then the silicon tetrachloride of the second cooling is supplied in the second refrigerating unit 230, thereby can obtain silicon tetrachloride product, the heat of the second tower bottoms is supplied to first heater simultaneously, by two-direction heat-exchanging, obtain the second tower bottoms of cooling, then the second tower bottoms of cooling is supplied in the 3rd refrigerating unit 110, thereby can obtain trichlorosilane products, above resulting liquid light constituent is supplied in the first refrigerating unit 600 simultaneously, thereby can obtain dichloro-dihydro silicon.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means to be contained at least one embodiment of the present invention or example in conjunction with specific features, structure, material or the feature of this embodiment or example description.In this manual, the schematic statement of above-mentioned term is not necessarily referred to identical embodiment or example.And the specific features of description, structure, material or feature can be with suitable mode combinations in any one or more embodiment or example.
Although illustrated and described embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, those of ordinary skill in the art can change above-described embodiment within the scope of the invention in the situation that not departing from principle of the present invention and aim, modification, replacement and modification.
Claims (10)
1. process a system for polycrystalline silicon tail gas dry reclaimed materials, described reclaimed materials contains dichloro-dihydro silicon, trichlorosilane and silicon tetrachloride, it is characterized in that, comprising:
First heater, described first heater is suitable for described reclaimed materials to carry out the first heat treated, to obtain the reclaimed materials through the first heat treated;
The second heating unit, described the second heating unit is connected with described first heater, and is suitable for the described reclaimed materials through the first heat treated to carry out the second heat treated, to obtain the reclaimed materials through the second heat treated;
The first rectification cell, described the first rectification cell is connected with described the second heating unit, and be suitable for the described reclaimed materials through the second heat treated to carry out the first rectification process, to obtain the first overhead vapours and the first tower bottoms, described the first tower bottoms contains silicon tetrachloride, and using described the first tower bottoms as thermal source, be back to described the second heating unit, to obtain silicon tetrachloride; And
The second rectifier unit, described the second rectifier unit is connected with described the first rectification cell, and be suitable for described the first overhead vapours to carry out the second rectification process, to obtain liquid light constituent and the second tower bottoms, described the second tower bottoms contains trichlorosilane, and described the second tower bottoms is back to described first heater as thermal source, to obtain trichlorosilane.
2. the system of processing polycrystalline silicon tail gas dry reclaimed materials according to claim 1, is characterized in that, further comprises:
Surge tank, described surge tank is connected with described the second rectifier unit with described the first rectification cell, and before being suitable for being stored in and carrying out described the second rectification process, thermal source using described the first overhead vapours as described the second rectifier unit and the overhead vapours phlegma that obtains, and a part for described overhead vapours phlegma is back to described the first rectification cell, and another part of described overhead vapours phlegma is passed into described the second rectifier unit.
3. the system of processing polycrystalline silicon tail gas dry reclaimed materials according to claim 2, is characterized in that, described the second heating unit further comprises:
The 3rd heating unit, described the 3rd heating unit is connected with described first heater, and is suitable for the described reclaimed materials through the first heat treated to carry out the 3rd heat treated, to obtain the reclaimed materials through the 3rd heat treated; And
The 4th heating unit, described the 4th heating unit is connected with described the 3rd heating unit, and is suitable for the described reclaimed materials through the 3rd heat treated to carry out the 4th heat treated, to obtain the described reclaimed materials through the second heat treated.
4. the system of processing polycrystalline silicon tail gas dry reclaimed materials according to claim 3, is characterized in that, described the first rectification cell further comprises:
The 3rd rectifier unit, described the 3rd rectifier unit is connected with described the 4th heating unit, and is suitable for a part for the described reclaimed materials through the second heat treated to carry out the 3rd rectification process, to obtain the 3rd overhead vapours and the 3rd tower bottoms; And
The 4th rectifier unit, described the 4th rectifier unit is connected with described the 4th heating unit, and is suitable for another part of the described reclaimed materials through the second heat treated to carry out the 4th rectification process, to obtain the 4th overhead vapours and the 4th tower bottoms.
5. the system of processing polycrystalline silicon tail gas dry reclaimed materials according to claim 1, is characterized in that, further comprises:
The first refrigerating unit, described the first refrigerating unit is connected with described the second rectifier unit, and is suitable for described liquid light constituent to carry out the first cooling process, so that separation obtains dichloro-dihydro silicon.
6. the system of processing polycrystalline silicon tail gas dry reclaimed materials according to claim 4, it is characterized in that, described surge tank is connected with described the second rectifier unit with described the 3rd rectifier unit, described the 4th rectifier unit respectively, and be suitable for the first part of described overhead vapours phlegma to be back to described the 3rd rectifier unit, the second section of described overhead vapours phlegma is back to described the 4th rectifier unit, the third part of described overhead vapours phlegma is passed into described the second rectifier unit.
7. the system of processing polycrystalline silicon tail gas dry reclaimed materials according to claim 4, it is characterized in that, described the 3rd rectifier unit is connected with the shell side opening for feed on described the 4th heating unit respectively with described the 4th rectifier unit, and be suitable for described the 3rd tower bottoms and described the 4th tower bottoms one of at least as thermal source, to be back to described the 4th heating unit, to obtain the silicon tetrachloride of the first cooling, shell side discharge port on described the 4th heating unit is connected with the shell side opening for feed on described the 3rd heating unit, and be suitable for the silicon tetrachloride of described the first cooling to be back to described the 3rd heating unit as thermal source, to obtain the silicon tetrachloride of the second cooling.
8. the system of processing polycrystalline silicon tail gas dry reclaimed materials according to claim 7, is characterized in that, further comprises:
The second refrigerating unit, described the second refrigerating unit is connected with described the 3rd heating unit, and is suitable for the silicon tetrachloride of described the second cooling to carry out the second cooling process, to obtain described silicon tetrachloride.
9. the system of processing polycrystalline silicon tail gas dry reclaimed materials according to claim 1, it is characterized in that, described the second rectifier unit is connected with described first heater, and be suitable for described the second tower bottoms to be back to described first heater as thermal source, to obtain the second tower bottoms of cooling.
10. the system of processing polycrystalline silicon tail gas dry reclaimed materials according to claim 9, is characterized in that, further comprises:
The 3rd refrigerating unit, described the 3rd refrigerating unit is connected with described the second rectifier unit, and is suitable for the second tower bottoms of described cooling to carry out the 3rd cooling process, to obtain trichlorosilane.
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Effective date of registration: 20201019 Address after: 100038 Fuxing Road 12, Beijing, Haidian District Patentee after: China Enfi Engineering Corp. Patentee after: CHINA SILICON Corp.,Ltd. Address before: 100038 Fuxing Road 12, Beijing, Haidian District Patentee before: China Enfi Engineering Corp. |