CN208130781U - The system for handling polycrystalline silicon reduction exhaust - Google Patents
The system for handling polycrystalline silicon reduction exhaust Download PDFInfo
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- CN208130781U CN208130781U CN201820008881.5U CN201820008881U CN208130781U CN 208130781 U CN208130781 U CN 208130781U CN 201820008881 U CN201820008881 U CN 201820008881U CN 208130781 U CN208130781 U CN 208130781U
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Abstract
The utility model discloses the systems of processing polycrystalline silicon reduction exhaust.The system includes：Absorption tower, the absorption tower have polycrystalline silicon reduction exhaust entrance, silicon tetrachloride entrance, hydrogen outlet and containing hydrogen chloride rich solution outlet；Rectifying column, the rectifying column have containing hydrogen chloride rich solution entrance, the outlet of the first chlorine hydride mixed gas, the outlet of recycling silicon tetrachloride and high-boiling components outlet；First segregator, first segregator have the first chlorine hydride mixed gas entrance, the outlet of the second chlorine hydride mixed gas and trichlorosilane outlet；Second segregator, second segregator have the second chlorine hydride mixed gas entrance, hydrogen chloride outlet and dichlorosilane outlet.The system uses silicon tetrachloride as absorbent absorbing hydrogen chloride, and by carrying out rectifying to containing hydrogen chloride rich solution, the separation of hydrogen chloride, silicon tetrachloride and high-boiling components, greatly simplification of flowsheet can be realized, achieved the purpose that efficient, energy conservation, reduced and invest.
Description
Technical field
The utility model relates to chemical fields, specifically, the utility model relates to handle polycrystalline silicon reduction exhaust to be
System.
Background technique
Generation hydrogen chloride tail gas, which uses, in polycrystalline reduction reaction at present the processes such as condenses, compresses, absorbs, desorbs, adsorbs
Chlorosilane, hydrogen chloride, hydrogen etc. in reduction tail gas are effectively separated, the chlorosilane after separation also needs to be sent to rectification working process
Two stage rectification is carried out, silicon tetrachloride and silicon powder therein can be just removed.
Application No. is 201610300902.6, the patent of entitled " polycrystalline silicon reduction exhaust recovery method and recovery system "
A kind of polycrystalline silicon reduction exhaust recovery method is provided, including：Utilize the cooling capacity of the fixed gas of hydrogen chloride absorption column overhead output
Cooling treatment is carried out to the reduction tail gas, obtains reduction tail gas after cooling；Using tower top from upper in hydrogen chloride absorption tower
The liquid-phase chlorosilane containing micro hydrogen chloride under and carries out absorption processing to the reduction tail gas after cooling, exports from tower reactor
Liquid-phase chlorosilane rich in hydrogen chloride exports fixed gas from tower top；It is defeated to hydrogen chloride absorption tower tower reactor in hydrogen chloride desorption tower
The liquid-phase chlorosilane rich in hydrogen chloride out carries out desorption processing；Using hydrogen chloride absorption tower tower reactor output rich in hydrogen chloride
The cooling capacity of liquid-phase chlorosilane carries out cooling treatment to the liquid-phase chlorosilane containing micro hydrogen chloride that hydrogen chloride desorption tower exports, and
The liquid-phase chlorosilane for containing micro hydrogen chloride after cooling is sent into hydrogen chloride absorption column overhead.Correspondingly, a kind of recycling is also provided
System.Recovery method described in the utility model and the cryogenic energy utilization of recovery system are reasonable.Process above is in classical absorption-
Desorption tail gas recycle technically optimizes heat balance, rationally utilizes cooling capacity, does not reduce process flow and equipment investment.
Therefore, the means of existing processing polycrystalline reduction gas still have much room for improvement.
Utility model content
The utility model is intended to solve at least some of the technical problems in related technologies.For this purpose, this reality
It is the system for proposing processing polycrystalline reduction gas with a novel purpose.The system is inhaled using silicon tetrachloride as absorbent
Hydrogen chloride is received, and by the way that the separation of hydrogen chloride, silicon tetrachloride and high-boiling components can be realized to the progress rectifying of containing hydrogen chloride rich solution,
Greatly simplification of flowsheet has achieved the purpose that efficient, energy conservation, has reduced investment.
In the one aspect of the utility model, the utility model proposes a kind of systems for handling polycrystalline silicon reduction exhaust.
Embodiment according to the present utility model, the system include：Absorption tower, the absorption tower have polycrystalline silicon reduction exhaust entrance, four
Silicon chloride entrance, hydrogen outlet and containing hydrogen chloride rich solution outlet；Rectifying column, the rectifying column have containing hydrogen chloride rich solution entrance,
First chlorine hydride mixed gas outlet, recycling silicon tetrachloride outlet and high-boiling components outlet, the containing hydrogen chloride rich solution entrance with it is described
Containing hydrogen chloride rich solution outlet is connected；First segregator, first segregator have the first chlorine hydride mixed gas entrance, the second chlorine
Change hydrogen mixed gas outlet and trichlorosilane outlet, the first chlorine hydride mixed gas entrance goes out with first chlorine hydride mixed gas
Mouth is connected；Second segregator, second segregator have the second chlorine hydride mixed gas entrance, hydrogen chloride outlet and dichloro-dihydro
Silicon outlet, the second chlorine hydride mixed gas entrance are connected with second chlorine hydride mixed gas outlet.
According to the system of the processing reduction tail gas of the utility model embodiment, by by polycrystalline silicon reduction exhaust and four chlorinations
Silicon is supplied to absorption tower, is absorbed using the silicon tetrachloride of high-purity to hydrogen chloride, since hydrogen chloride is in silicon tetrachloride
Solubility it is higher, it can be ensured that better assimilation effect, and reduce absorbent dosage obtains containing hydrogen chloride rich solution, and separate
Obtained hydrogen；Subsequent supply containing hydrogen chloride rich solution into rectifying column carries out rectification process, using a rectifying column simultaneously into
The rectifying of the desorption of hydrogen chloride and chlorosilane in row rich solution can be realized high boiling to hydrogen chloride, silicon tetrachloride and silicon powder, impurity etc.
The separation of object, using the function of a desorber in rectifying column substitution traditional handicraft, two rectifying columns, and in rectifying tower
Top obtains the first chlorine hydride mixed gas, recycles to obtain silicon tetrachloride in tower reactor, while greatly simplification of flowsheet, may be used also
The load of subsequent technique is effectively reduced；Further, the first chlorine hydride mixed gas is supplied to segregate into the first segregator and is removed
Trichlorosilane is removed, and obtains the second chlorine hydride mixed gas；Second chlorine hydride mixed gas is supplied to segregate into the second segregator and is removed
Dichlorosilane is gone, to obtain hydrogen chloride gas.The system of the processing polycrystalline silicon reduction exhaust of the utility model uses as a result,
Silicon tetrachloride carries out rectifying to containing hydrogen chloride rich solution as absorbent absorbing hydrogen chloride, and by a rectifying column, can be realized
The separation of hydrogen chloride, silicon tetrachloride and high-boiling components, greatly simplification of flowsheet have reached efficient, energy conservation, the mesh for reducing investment
's.
Optional, the system of the processing polycrystalline silicon reduction exhaust further comprises：Storage tank, the storage tank have trichlorine hydrogen
Silicon entrance and the outlet of recycling trichlorosilane；The rectifying column also has recycling trichlorosilane entrance, and the recycling trichlorosilane enters
Mouth is connected with recycling trichlorosilane outlet.Thus, it is possible to the trichlorosilane supply tank that the first segregator is segregated
In keep in, the trichlorosilane being collected into can return in rectifying column for rectification process, can also enter subsequent rectifying purification process.
Optional, the system of the processing polycrystalline silicon reduction exhaust further comprises：First Heat Exchanger, first heat exchange
There is device the first high temperature silicon tetrachloride entrance and the first low temperature silicon tetrachloride to export, the first high temperature silicon tetrachloride entrance and institute
The outlet of recycling silicon tetrachloride is stated to be connected；Second heat exchanger, second heat exchanger have the second high temperature silicon tetrachloride entrance, low temperature
Containing hydrogen chloride rich solution entrance, the outlet of the second low temperature silicon tetrachloride and high temperature containing hydrogen chloride rich solution outlet, the second high temperature tetrachloro
SiClx entrance is connected with the first low temperature silicon tetrachloride outlet, the low temperature containing hydrogen chloride rich solution entrance and the absorption tower
Containing hydrogen chloride rich solution outlet is connected, and high temperature containing hydrogen chloride rich solution outlet is connected with the containing hydrogen chloride rich solution entrance of rectifying column.As a result,
Containing hydrogen chloride rich solution in absorption tower enters back into rectifying column after can preheating with recovered silicon tetrachloride, so as to further increase
The heat utilization efficiency of technique.
Optional, the second low temperature silicon tetrachloride outlet is connected with the silicon tetrachloride entrance on the absorption tower.It is smart as a result,
Evaporating the silicon tetrachloride that tower recycles can return in absorption tower after two-stage exchanges heat for the absorption to polycrystalline silicon reduction exhaust.
The additional aspect and advantage of the utility model will be set forth in part in the description, partially will be from following description
In become obvious, or recognized by the practice of the utility model.
Detailed description of the invention
The above-mentioned and/or additional aspect and advantage of the utility model from the description of the embodiment in conjunction with the following figures will
Become obvious and is readily appreciated that, wherein：
Fig. 1 is the system structure diagram according to the processing polycrystalline silicon reduction exhaust of the utility model one embodiment；
Fig. 2 is the system structure diagram according to the processing polycrystalline silicon reduction exhaust of the utility model further embodiment；
Fig. 3 is the system structure diagram according to the processing polycrystalline silicon reduction exhaust of the utility model another embodiment；
Fig. 4 is the system processing polycrystalline reduction using the processing polycrystalline silicon reduction exhaust of the utility model one embodiment
The method flow schematic diagram of tail gas；
Fig. 5 is to handle polysilicon also using the system of the processing polycrystalline silicon reduction exhaust of the utility model further embodiment
The method flow schematic diagram of protocercal tail gas；
Fig. 6 is to handle polysilicon also using the system of the processing polycrystalline silicon reduction exhaust of another embodiment of the utility model
The method flow schematic diagram of protocercal tail gas.
Specific embodiment
The embodiments of the present invention are described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning
Same or similar element or element with the same or similar functions are indicated to same or similar label eventually.Below by ginseng
The embodiment for examining attached drawing description is exemplary, it is intended to for explaining the utility model, and should not be understood as to the utility model
Limitation.
In the description of the present invention, it should be understood that term " on ", "lower", "front", "rear", "left", "right",
The orientation or positional relationship of the instructions such as "vertical", "horizontal", "top", "bottom", "inner", "outside" be orientation based on the figure or
Positional relationship is merely for convenience of describing the present invention and simplifying the description, rather than the device or member of indication or suggestion meaning
Part must have a particular orientation, be constructed and operated in a specific orientation, therefore should not be understood as limiting the present invention.
In addition, term " first ", " second " are used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance
Or implicitly indicate the quantity of indicated technical characteristic.Define " first " as a result, the feature of " second " can be expressed or
Implicitly include at least one this feature.The meaning of " plurality " is at least two, such as two in the description of the present invention,
It is a, three etc., unless otherwise specifically defined.
In the present invention unless specifically defined or limited otherwise, the terms such as " connected ", " connection ", " fixation " are answered
It is interpreted broadly, for example, it may be being fixedly connected, may be a detachable connection, or is integral；It can be mechanical connection,
It can be electrical connection；It can be directly connected, the company inside two elements can also be can be indirectly connected through an intermediary
Logical or two elements interaction relationship, unless otherwise restricted clearly.For the ordinary skill in the art, may be used
To understand the concrete meaning of above-mentioned term in the present invention as the case may be.
In the present invention unless specifically defined or limited otherwise, fisrt feature is in the second feature " on " or " down "
It can be that the first and second features directly contact or the first and second features are by intermediary mediate contact.Moreover, first is special
Sign can be fisrt feature above the second feature " above ", " above " and " above " and be directly above or diagonally above the second feature, or only
Indicate that first feature horizontal height is higher than second feature.Fisrt feature under the second feature " below ", " below " and " below " can be with
It is that fisrt feature is directly under or diagonally below the second feature, or is merely representative of first feature horizontal height less than second feature.
In the one aspect of the utility model, the utility model proposes a kind of systems for handling polycrystalline silicon reduction exhaust.
Embodiment according to the present utility model, with reference to Fig. 1~3, which includes：Absorption tower 100, rectifying column 200, the first segregator
300 and second segregator 400.Wherein, absorption tower 100 have polycrystalline silicon reduction exhaust entrance 101, silicon tetrachloride entrance 102,
Hydrogen outlet 103 and containing hydrogen chloride rich solution outlet 104；Rectifying column 200 has containing hydrogen chloride rich solution entrance 201, the first hydrogen chloride
Mixed gas outlet 202, recycling silicon tetrachloride outlet 203 and high-boiling components outlet 204, containing hydrogen chloride rich solution entrance 201 and chloride containing
Hydrogen rich solution outlet 104 is connected；There is first segregator 300 first chlorine hydride mixed gas entrance 301, the second chlorine hydride mixed gas to go out
Mouth 302 and trichlorosilane outlet 303, the first chlorine hydride mixed gas entrance 301 are connected with the first chlorine hydride mixed gas outlet 202；
Second segregator 400 has the second chlorine hydride mixed gas entrance 401, hydrogen chloride outlet 402 and dichlorosilane outlet 403, the
Dichloride hydrogen gaseous mixture entrance 401 is connected with the second chlorine hydride mixed gas outlet 302.
According to the system of the processing reduction tail gas of the utility model embodiment, by by polycrystalline silicon reduction exhaust and four chlorinations
Silicon is supplied to absorption tower, is absorbed using the silicon tetrachloride of high-purity to hydrogen chloride, since hydrogen chloride is in silicon tetrachloride
Solubility it is higher, it can be ensured that better assimilation effect, and reduce absorbent dosage obtains containing hydrogen chloride rich solution, and separate
Obtained hydrogen；Subsequent supply containing hydrogen chloride rich solution into rectifying column carries out rectification process, using a rectifying column simultaneously into
The rectifying of the desorption of hydrogen chloride and chlorosilane in row rich solution can be realized high boiling to hydrogen chloride, silicon tetrachloride and silicon powder, impurity etc.
The separation of object, using the function of a desorber in rectifying column substitution traditional handicraft, two rectifying columns, and in rectifying tower
Top obtains the first chlorine hydride mixed gas, recycles to obtain silicon tetrachloride in tower reactor, while greatly simplification of flowsheet, may be used also
The load of subsequent technique is effectively reduced；Further, the first chlorine hydride mixed gas is supplied to segregate into the first segregator and is removed
Trichlorosilane is removed, and obtains the second chlorine hydride mixed gas；Second chlorine hydride mixed gas is supplied to segregate into the second segregator and is removed
Dichlorosilane is gone, to obtain hydrogen chloride gas.The system of the processing polycrystalline silicon reduction exhaust of the utility model uses as a result,
Silicon tetrachloride carries out rectifying to containing hydrogen chloride rich solution as absorbent absorbing hydrogen chloride, and by a rectifying column, can be realized
The separation of hydrogen chloride, silicon tetrachloride and high-boiling components, greatly simplification of flowsheet have reached efficient, energy conservation, the mesh for reducing investment
's.
It is carried out in detail below with reference to Fig. 1~3 pair according to the system of the processing polycrystalline silicon reduction exhaust of the utility model embodiment
Thin description：
There is polycrystalline silicon reduction exhaust entrance 101, silicon tetrachloride to enter for embodiment according to the present utility model, absorption tower 100
Mouth 102, hydrogen outlet 103 and containing hydrogen chloride rich solution outlet 104, absorption tower 100 are suitable for polycrystalline silicon reduction exhaust and four chlorinations
Silicon carries out absorption processing, to obtain containing hydrogen chloride rich solution, and isolated hydrogen.Containing a large amount of in polycrystalline silicon reduction exhaust
Hydrogen, trichlorosilane and the chlorosilane cpds such as byproduct of reaction hydrogen chloride and dichlorosilane.What the utility model used
The silicon tetrachloride of high-purity absorbs the hydrogen chloride in polycrystalline silicon reduction exhaust, since hydrogen chloride is molten in silicon tetrachloride
Du Genggao is solved, boiling point is higher, it can be ensured that better assimilation effect, and the dosage of absorbent is reduced, it can also make to separate as a result,
Contain less silicon tetrachloride in obtained hydrogen, reduces the device load of hydrogen subsequent adsorbtion process.
Specific embodiment according to the present utility model, the tower top temperature on absorption tower are -40~-37 DEG C, tower top pressure 1.0
~1.1 MPa, bottom temperature are -35~-32 DEG C, and tower reactor pressure is 1.0~1.1MPa.Thus, it is possible to further be conducive to four
Absorption of the silicon chloride to hydrogen chloride, and further decrease the content of hydrogen chloride and silicon tetrachloride in isolated hydrogen.
Embodiment according to the present utility model, rectifying column 200 have containing hydrogen chloride rich solution entrance 201, the first hydrogen chloride mixed
Close gas outlet 202, recycling silicon tetrachloride outlet 203 and high-boiling components outlet 204, containing hydrogen chloride rich solution entrance 201 and containing hydrogen chloride
Rich solution outlet 104 is connected, and rectifying column 200 is suitable for containing hydrogen chloride rich solution carrying out rectification process, mixed to obtain the first hydrogen chloride
Close gas, recycling silicon tetrachloride and high-boiling components.Embodiment according to the present utility model supplies containing hydrogen chloride rich solution into rectifying column
Rectification process is carried out, the rectifying of the desorption of hydrogen chloride and chlorosilane in rich solution is carried out simultaneously using a rectifying column, can be realized
Separation to the high-boiling components such as hydrogen chloride, silicon tetrachloride and silicon powder, impurity, using a solution in a rectifying column substitution traditional handicraft
The function of tower, two rectifying columns is inhaled, and obtains the first chlorine hydride mixed gas in the top of the distillation column, recycles to obtain four chlorinations in tower reactor
While greatly simplification of flowsheet the load of subsequent technique can also be effectively reduced, it is high boiling that tower reactor produces silicon powder etc. in silicon
Object impurity can be sent to slurry recovery system.On the other hand, the utility model recycles to obtain the first hydrogen chloride in the top of the distillation column
The gas phase recovery process of gaseous mixture can also save a large amount of cooling capacity relative to Traditional liquid phase recovery process.
Specific embodiment according to the present utility model, the tower top temperature of rectifying column are 79~81 DEG C, tower top pressure 0.35
~0.36 MPa, bottom temperature are 115~117 DEG C, and tower reactor pressure is 0.39~0.40MPa.Existing absorption-desorption technique
In, rectifying tower pressure on top surface in 1.0MPa or so, the utility model by by the setting of rectifying tower pressure on top surface 0.35~
0.36MPa can make the hydrogen chloride in chlorosilane be easier to carry out desorbing, so that the dosage of tower reactor steam is reduced, in combination with
Above-mentioned tower top temperature, bottom temperature and tower reactor pressure parameter can further be conducive to the desorption of hydrogen chloride, improve hydrogen chloride
The rate of recovery.
Embodiment according to the present utility model, the first segregator 300 have the first chlorine hydride mixed gas entrance 301, second
Chlorine hydride mixed gas outlet 302 and trichlorosilane outlet 303, the first chlorine hydride mixed gas entrance 301 is mixed with the first hydrogen chloride
Gas outlet 202 is connected, and the first segregator 300 is suitable for the first chlorine hydride mixed gas carrying out the first fractional condensation processing, to obtain the
Dichloride hydrogen gaseous mixture and trichlorosilane.
With reference to Fig. 2, the system of the processing polycrystalline silicon reduction exhaust of the utility model be can further include：Storage tank 500.
Embodiment according to the present utility model, storage tank 500 have trichlorosilane entrance 501 and the outlet of recycling trichlorosilane
502；Rectifying column 200 also has recycling trichlorosilane entrance 205, recycling trichlorosilane entrance 205 and the outlet of recycling trichlorosilane
502 are connected.Thus, it is possible to be kept in the trichlorosilane supply tank that the first segregator is segregated, the trichlorine hydrogen being collected into
Silicon a part returns and is used for rectification process in rectifying column, and another part enters subsequent trichlorosilane rectification and purification process.Return to essence
A part of trichlorosilane for evaporating tower can carry out heat transfer and mass transfer with the trichlorosilane steam risen in rectifying column, to realize back
Receive point of light component and heavy constituent in trichlorosilane gas in light component and heavy constituent and the rectifying column in trichlorosilane liquid
From.
Specific embodiment according to the present utility model, recycling trichlorosilane entrance 205 export 502 phases with recycling trichlorosilane
It can be even connected by delivery pump.
Embodiment according to the present utility model, the second segregator 400 have the second chlorine hydride mixed gas entrance 401, chlorination
Hydrogen outlet 402 and dichlorosilane outlet 403, the second chlorine hydride mixed gas entrance 401 and the second chlorine hydride mixed gas outlet 302
It is connected, the second segregator 400 is suitable for the second chlorine hydride mixed gas carrying out the second fractional condensation processing, to obtain hydrogen chloride and dichloro
Dihydro silicon, wherein isolated dichlorosilane can be sent to anti-disproportionation process and be used.
With reference to Fig. 3, the system of the processing polycrystalline silicon reduction exhaust of the utility model be can further include：First heat exchange
Device 600 and the second heat exchanger 700.
Embodiment according to the present utility model, First Heat Exchanger 600 have the first high temperature silicon tetrachloride entrance 601 and first
Low temperature silicon tetrachloride outlet 602, the recycling silicon tetrachloride outlet 203 of the first high temperature silicon tetrachloride entrance 601 and rectifying column 200
It is connected.The silicon tetrachloride recycled in rectifying column as a result, can first cool down in First Heat Exchanger, and first obtained is low
Warm silicon tetrachloride can send to cold hydrogenation process and be used, and can also supply to the second heat exchanger 700 and be used for containing hydrogen chloride
Rich solution is preheated.
Embodiment according to the present utility model, the second heat exchanger 700 have the second high temperature silicon tetrachloride entrance 701, low temperature
Containing hydrogen chloride rich solution entrance 702, the second low temperature silicon tetrachloride outlet 703 and high temperature containing hydrogen chloride rich solution outlet 704, the second high temperature
Silicon tetrachloride entrance 701 is connected with the first low temperature silicon tetrachloride outlet 602, low temperature containing hydrogen chloride rich solution entrance 702 and absorption tower
100 containing hydrogen chloride rich solution outlet 104 is connected, the containing hydrogen chloride rich solution of high temperature containing hydrogen chloride rich solution outlet 704 and rectifying column 200
Entrance 201 is connected.Thus, it is possible to supply containing hydrogen chloride rich solution obtained in absorption tower into the second heat exchanger, make chloride containing
Rectifying column is entered back into after the recovered silicon tetrachloride preheating of hydrogen rich solution, so as to further increase the heat utilization efficiency of technique.
Specific embodiment according to the present utility model, the second high temperature silicon tetrachloride entrance 701 and the first low temperature silicon tetrachloride
Conveying can be passed through between outlet 602 and between low temperature containing hydrogen chloride rich solution entrance 702 and containing hydrogen chloride rich solution outlet 104
Pump is connected.
Specific embodiment according to the present utility model, four chlorinations of the second low temperature silicon tetrachloride outlet 703 and absorption tower 100
Silicon entrance 102 is connected.The silicon tetrachloride that rectifying column recycles as a result, is can return in absorption tower after two-stage exchanges heat for more
The absorption of crystal silicon reduction tail gas.
In order to facilitate understanding, below with reference to Fig. 4~6 pair using the processing polycrystalline silicon reduction exhaust of the utility model embodiment
System processing polycrystalline silicon reduction exhaust method be described in detail.Embodiment according to the present utility model, this method include：
S100：Absorption processing
In the step, polycrystalline silicon reduction exhaust and silicon tetrachloride are supplied into absorption tower and carry out absorption processing, so as to
To containing hydrogen chloride rich solution, and isolated hydrogen.It is secondary containing a large amount of hydrogen, trichlorosilane and reaction in polycrystalline silicon reduction exhaust
The chlorosilane cpds such as product hydrogen chloride and dichlorosilane.The silicon tetrachloride for the high-purity that the utility model uses is to polysilicon
Hydrogen chloride in reduction tail gas is absorbed, and since solubility of the hydrogen chloride in silicon tetrachloride is higher, boiling point is higher, can be true
Better assimilation effect is protected, and reduces the dosage of absorbent, can also make to contain less four in isolated hydrogen as a result,
Silicon chloride reduces the device load of hydrogen subsequent adsorbtion process.
Specific embodiment according to the present utility model, the tower top temperature on absorption tower are -40~-37 DEG C, tower top pressure 1.0
~1.1 MPa, bottom temperature are -35~-32 DEG C, and tower reactor pressure is 1.0~1.1MPa.Thus, it is possible to further be conducive to four
Absorption of the silicon chloride to hydrogen chloride, and further decrease the content of hydrogen chloride and silicon tetrachloride in isolated hydrogen.
S200：Rectification process
In the step, containing hydrogen chloride rich solution is supplied into rectifying column and carries out rectification process, to obtain the first hydrogen chloride
Gaseous mixture, recycling silicon tetrachloride and high-boiling components.Embodiment according to the present utility model supplies containing hydrogen chloride rich solution to rectifying column
Middle carry out rectification process carries out the rectifying of the desorption of hydrogen chloride and chlorosilane in rich solution, Ji Keshi using a rectifying column simultaneously
Now to the separation of the high-boiling components such as hydrogen chloride, silicon tetrachloride and silicon powder, impurity, using one in a rectifying column substitution traditional handicraft
The function of desorber, two rectifying columns, and the first chlorine hydride mixed gas is obtained in the top of the distillation column, it recycles to obtain tetrachloro in tower reactor
While greatly simplification of flowsheet the load of subsequent technique can also be effectively reduced, it is contour that tower reactor produces silicon powder in SiClx
Boiling object impurity can be sent to slurry recovery system.On the other hand, the utility model recycles to obtain the first chlorination in the top of the distillation column
The gas phase recovery process of hydrogen gaseous mixture can also save a large amount of cooling capacity relative to Traditional liquid phase recovery process.
Specific embodiment according to the present utility model, the tower top temperature of rectifying column are 79~81 DEG C, tower top pressure 0.35
~0.36 MPa, bottom temperature are 115~117 DEG C, and tower reactor pressure is 0.39~0.40MPa.Existing absorption-desorption technique
In, rectifying tower pressure on top surface in 1.0MPa or so, the utility model by by the setting of rectifying tower pressure on top surface 0.35~
0.36MPa can make the hydrogen chloride in chlorosilane be easier to carry out desorbing, so that the dosage of tower reactor steam is reduced, in combination with
Above-mentioned tower top temperature, bottom temperature and tower reactor pressure parameter can further be conducive to the desorption of hydrogen chloride, improve hydrogen chloride
The rate of recovery.
S300：First fractional condensation processing
In the step, the first chlorine hydride mixed gas is supplied and carries out the first fractional condensation processing into the first segregator, so as to
To the second chlorine hydride mixed gas and trichlorosilane.
With reference to Fig. 5, the method for the processing polycrystalline silicon reduction exhaust of the utility model be can further include：By trichlorine hydrogen
Silicon is supplied to be stored into storage tank, and trichlorosilane a part for being collected into returns in rectifying column for rectification process, another part into
Enter subsequent trichlorosilane rectification and purification process.A part of trichlorosilane for returning to rectifying column can be with the trichlorine that rises in rectifying column
Hydrogen silicon steam carries out heat transfer and mass transfer, to realize the light component and heavy constituent and rectifying column in recycling trichlorosilane liquid
The separation of light component and heavy constituent in interior trichlorosilane gas.
S400：Second fractional condensation processing
In the step, the second chlorine hydride mixed gas is supplied and carries out the second fractional condensation processing into the second segregator, so as to
To hydrogen chloride and dichlorosilane.
With reference to Fig. 6, the method for the processing polycrystalline silicon reduction exhaust of the utility model be can further include：
Recycling silicon tetrachloride is supplied and is exchanged heat into First Heat Exchanger, to obtain the first low temperature silicon tetrachloride；By
This, the silicon tetrachloride recycled in rectifying column can first cool down in First Heat Exchanger, the first obtained low temperature tetrachloro
SiClx can be sent to cold hydrogenation process and be used, can also supply to the second heat exchanger 700 be used for containing hydrogen chloride rich solution into
Row preheating.
A part supply of first low temperature silicon tetrachloride is changed into the second heat exchanger with the containing hydrogen chloride rich solution
Heat, to obtain high temperature containing hydrogen chloride rich solution and the second low temperature silicon tetrachloride.Thus, it is possible to by chloride containing obtained in absorption tower
Hydrogen rich solution is supplied into the second heat exchanger, enters back into rectifying column after making the recovered silicon tetrachloride preheating of containing hydrogen chloride rich solution, thus
It can be further improved the heat utilization efficiency of technique.
Second low temperature silicon tetrachloride can also be returned in the absorption tower and be used by specific embodiment according to the present utility model
It is handled in absorption.
According to the method for the processing reduction tail gas of the utility model embodiment, by by polycrystalline silicon reduction exhaust and four chlorinations
Silicon is supplied to absorption tower, is absorbed using the silicon tetrachloride of high-purity to hydrogen chloride, since hydrogen chloride is in silicon tetrachloride
Solubility it is higher, it can be ensured that better assimilation effect, and reduce absorbent dosage obtains containing hydrogen chloride rich solution, and separate
Obtained hydrogen；Subsequent supply containing hydrogen chloride rich solution into rectifying column carries out rectification process, using a rectifying column simultaneously into
The rectifying of the desorption of hydrogen chloride and chlorosilane in row rich solution can be realized high boiling to hydrogen chloride, silicon tetrachloride and silicon powder, impurity etc.
The separation of object, using the function of a desorber in rectifying column substitution traditional handicraft, two rectifying columns, and in rectifying tower
Top obtains the first chlorine hydride mixed gas, recycles to obtain silicon tetrachloride in tower reactor, while greatly simplification of flowsheet, may be used also
The load of subsequent technique is effectively reduced；Further, the first chlorine hydride mixed gas is supplied to segregate into the first segregator and is removed
Trichlorosilane is removed, and obtains the second chlorine hydride mixed gas；Second chlorine hydride mixed gas is supplied to segregate into the second segregator and is removed
Dichlorosilane is gone, to obtain hydrogen chloride gas.The method of the processing polycrystalline silicon reduction exhaust of the utility model uses as a result,
Silicon tetrachloride carries out rectifying to containing hydrogen chloride rich solution as absorbent absorbing hydrogen chloride, and by a rectifying column, can be realized
The separation of hydrogen chloride, silicon tetrachloride and high-boiling components, greatly simplification of flowsheet have reached efficient, energy conservation, the mesh for reducing investment
's.
Below with reference to specific embodiment, the utility model is described, it should be noted that these embodiments are only
Descriptive, without limiting the utility model in any way.
Embodiment
Contain hydrogen, trichlorosilane, silicon tetrachloride, hydrogen chloride etc. in production of polysilicon tail gas.It is handled according to the following steps
Polycrystalline silicon reduction exhaust：
Polycrystalline silicon reduction exhaust and silicon tetrachloride are supplied into absorption tower and carry out absorption processing, to obtain containing hydrogen chloride
Rich solution, and isolated hydrogen；It is detected, H in obtained hydrogen2Content is not less than 99.5v%, and HCl content is not higher than
0.004v%, content of silicon tetrachloride are not higher than 0.001v%；
Containing hydrogen chloride rich solution is supplied into rectifying column and carries out rectification process, to obtain the first chlorine hydride mixed gas, to return
Receive silicon tetrachloride and high-boiling components；Wherein, it recycles content of silicon tetrachloride in silicon tetrachloride and is not less than 99wt%, high-boiling components content is not high
In 1wt%.
First chlorine hydride mixed gas is supplied and carries out the first fractional condensation processing into the first segregator, to obtain the second chlorination
Hydrogen gaseous mixture and trichlorosilane；It is detected, trichlorosilane content is not less than 94wt%, dichlorosilane in obtained trichlorosilane
Content is not higher than 6v%.
Second chlorine hydride mixed gas is supplied and carries out the second fractional condensation processing into the second segregator, so as to obtain hydrogen chloride and
Dichlorosilane；It is detected, HCl purity is not less than 60v%, H in obtained hydrogen chloride gas2Content is not higher than 39v%, trichlorine
Hydrogen silicone content is not higher than 0.01v%；
Trichlorosilane is supplied and is stored into storage tank, and a part of trichlorosilane is returned in rectifying column and is used at rectifying
Reason；
Recycling silicon tetrachloride is supplied and is exchanged heat into First Heat Exchanger, to obtain the first low temperature silicon tetrachloride；
A part supply of first low temperature silicon tetrachloride is exchanged heat into the second heat exchanger with containing hydrogen chloride rich solution, with
Just high temperature containing hydrogen chloride rich solution and the second low temperature silicon tetrachloride are obtained；
Second low temperature silicon tetrachloride is returned in absorption tower and is used to absorb processing.
Polycrystalline silicon reduction exhaust, H are handled according to above step2The rate of recovery is not less than not less than 99.2%, the HCl rate of recovery
99.3%, SiHCl3The rate of recovery is not less than 99.5%, SiCl4The rate of recovery is not less than 99.3%.
By taking a set of 3000 tons/year of polycrystalline silicon devices as an example.Polysilicon is handled also using the system and method for the utility model
Protocercal tail gas, it is possible to reduce absorption tower, silicon tetrachloride rectifying column and relevant device, pipeline, valve in traditional handicraft absorption-desorption technique
About 8,500,000 yuan of related investments of door etc..Desorber 2 × 6.7t/h of steam consumption can be reduced, silicon tetrachloride rectifying steam is reduced and uses
5.8t/h is measured, about 13,050,000 yuan of economic benefit is converted into.The technical program is total can to bring about 21,550,000 yuan of benefit.Such as ten thousand tons and
The above polycrystalline silicon device, this technology bring economic benefit will be multiplied.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is contained at least one embodiment or example of the utility model.In the present specification, to the schematic table of above-mentioned term
It states and is necessarily directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be with
It can be combined in any suitable manner in any one or more of the embodiments or examples.In addition, without conflicting with each other, this field
Technical staff can by the feature of different embodiments or examples described in this specification and different embodiments or examples into
Row combination and combination.
Although the embodiments of the present invention have been shown and described above, it is to be understood that above-described embodiment is
Illustratively, it should not be understood as limiting the present invention, those skilled in the art are in the scope of the utility model
Inside it can make changes, modifications, alterations, and variations to the above described embodiments.
Claims (4)
1. a kind of system for handling polycrystalline silicon reduction exhaust, which is characterized in that including：
Absorption tower, the absorption tower have polycrystalline silicon reduction exhaust entrance, silicon tetrachloride entrance, hydrogen outlet and containing hydrogen chloride rich
Liquid outlet；
There is containing hydrogen chloride rich solution entrance, the outlet of the first chlorine hydride mixed gas, recycling silicon tetrachloride to go out for rectifying column, the rectifying column
Mouth and high-boiling components outlet, the containing hydrogen chloride rich solution entrance are connected with the containing hydrogen chloride rich solution outlet；
First segregator, first segregator have the first chlorine hydride mixed gas entrance, the second chlorine hydride mixed gas outlet and
Trichlorosilane outlet, the first chlorine hydride mixed gas entrance are connected with first chlorine hydride mixed gas outlet；
Second segregator, second segregator have the second chlorine hydride mixed gas entrance, hydrogen chloride outlet and dichlorosilane
Outlet, the second chlorine hydride mixed gas entrance are connected with second chlorine hydride mixed gas outlet.
2. the system of processing polycrystalline silicon reduction exhaust according to claim 1, which is characterized in that further comprise：
Storage tank, the storage tank have trichlorosilane entrance and the outlet of recycling trichlorosilane；The rectifying column also has recycling trichlorine
Hydrogen silicon entrance, the recycling trichlorosilane entrance are connected with recycling trichlorosilane outlet.
3. the system of processing polycrystalline silicon reduction exhaust according to claim 1, which is characterized in that further comprise：
There is the first high temperature silicon tetrachloride entrance and the first low temperature silicon tetrachloride to export for First Heat Exchanger, the First Heat Exchanger,
The first high temperature silicon tetrachloride entrance is connected with recycling silicon tetrachloride outlet；
Second heat exchanger, second heat exchanger have the second high temperature silicon tetrachloride entrance, low temperature containing hydrogen chloride rich solution entrance, the
The outlet of two low temperature silicon tetrachlorides and high temperature containing hydrogen chloride rich solution outlet, the second high temperature silicon tetrachloride entrance are low with described first
Warm silicon tetrachloride outlet is connected, the containing hydrogen chloride rich solution outlet phase of the low temperature containing hydrogen chloride rich solution entrance and the absorption tower
Even, high temperature containing hydrogen chloride rich solution outlet is connected with the containing hydrogen chloride rich solution entrance of the rectifying column.
4. the system of processing polycrystalline silicon reduction exhaust according to claim 3, which is characterized in that the second low temperature tetrachloro
SiClx outlet is connected with the silicon tetrachloride entrance on the absorption tower.
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| CN201820008881.5U CN208130781U (en) | 2018-01-03 | 2018-01-03 | The system for handling polycrystalline silicon reduction exhaust |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109985489A (en) * | 2018-01-03 | 2019-07-09 | 国电内蒙古晶阳能源有限公司 | The system and method for handling polycrystalline silicon reduction exhaust |
| CN112138524A (en) * | 2019-06-28 | 2020-12-29 | 新特能源股份有限公司 | Purification method and purification system for tail gas of polycrystalline silicon reduction process |
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2018
- 2018-01-03 CN CN201820008881.5U patent/CN208130781U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109985489A (en) * | 2018-01-03 | 2019-07-09 | 国电内蒙古晶阳能源有限公司 | The system and method for handling polycrystalline silicon reduction exhaust |
| CN112138524A (en) * | 2019-06-28 | 2020-12-29 | 新特能源股份有限公司 | Purification method and purification system for tail gas of polycrystalline silicon reduction process |
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