CN108502889A - The separation of polysilicon cold hydrogenation product and purifying plant and method - Google Patents
The separation of polysilicon cold hydrogenation product and purifying plant and method Download PDFInfo
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- CN108502889A CN108502889A CN201810612483.9A CN201810612483A CN108502889A CN 108502889 A CN108502889 A CN 108502889A CN 201810612483 A CN201810612483 A CN 201810612483A CN 108502889 A CN108502889 A CN 108502889A
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Abstract
The invention discloses a kind of separation of polysilicon cold hydrogenation product and purifying plant and methods, the device includes level-one crude tower and two level crude tower, wherein, level-one crude tower does not detach STC, two level crude tower detaches STC, and for receiving cold hydrogenation product, the tower top outlet of level-one crude tower is connected to the feed(raw material)inlet of two level crude tower for the feed(raw material)inlet of level-one crude tower, the tower top outlet of two level crude tower is connected to the distillation system in downstream, and the kettle material of two level crude tower returns to cold hydrogenation apparatus；Above-mentioned apparatus rough segmentation purity is higher, can reduce the pressure of follow-up rectification process；It is only simultaneously a portion in raw material into the silicon tetrachloride of two level crude tower, therefore the minimum number of theoretical plate of two level crude tower can be less than the minimum number of theoretical plate of traditional crude tower in the prior art, namely the load and energy consumption of two level crude tower can be relatively low, the scale and input for contributing to reduction distillation system, to reduce fault in production rate.
Description
Technical field
The present invention relates to technical field of polysilicon production, more particularly to a kind of polysilicon cold hydrogenation product separation and purification dress
It sets and method.
Background technology
Improved Siemens are that the most widely used method for preparing high purity polycrystalline silicon, the product of this method remove in the world
Outside polysilicon, also not reacted trichlorosilane (TCS), a large amount of silicon tetrachlorides (STC), dichlorosilane (DCS), hydrogen chloride and
Hydrogen.For silicon tetrachloride after subsequent tail gas recycle, rectifying etc. are separated, hydro-conversion is that trichlorosilane returns to reduction furnace
It uses.
Currently, silicon tetrachloride hydro-conversion is mostly trichlorosilane using cold hydrogenation process by polysilicon factory, cold hydrogenation is anti-
By detaching and purifying after the product condensation answered, high-purity trichlorosilane is sent into reduction furnace carries out reaction and prepare polysilicon.It is cold
The content of trichlorosilane is generally less than 30% (mole) in hydrogenation product (the condensed material of reaction end gas), and the overwhelming majority is four
Silicon chloride, a small amount of dichlorosilane (being generally less than 1%), also contains the heavy constituents such as a small amount of high-boiling components.
1 explanation cold hydrogenation product rough segmentation and rectification and purification technological process in the prior art below in conjunction with the accompanying drawings, cold hydrogenation production
Product enter crude tower as raw material, and crude tower separates the silicon tetrachloride in material from tower reactor, and fixed gas is discharged from tower top,
Trichlorosilane and dichlorosilane then remove to enter subsequent 1# rectifying columns except light, 2# rectifying columns are except weight, 3# rectifying columns from overhead extraction
Except light, 4# rectifying columns are except weight.The silicon tetrachloride of rough segmentation tower reactor then passes through STC purifying columns and purifies, and the silicon tetrachloride of tower top cleaning is then
It returns to cold hydrogenation and continues hydroconversion reactions, useless silicon tetrachloride of the tower reactor containing a large amount of high-boiling components then sends to liquid waste processing progress
Subsequent hydrolysis or evaporation recovery processing.Simultaneously these above-mentioned rectifying columns can carry out heat coupling realize it is energy saving, heat couple when,
General couple column overhead temperatures can be realized higher than being coupled 20 DEG C of tower bottom temperature.Such as the tower-coupled 3# rectifying columns of 4# rectifying,
The tower-coupled 1# rectifying columns of 2# rectifying, STC purify the modes such as tower-coupled 4# rectifying columns, but because contain in the material of rough segmentation column overhead
A certain amount of dichlorosilane causes its saturation temperature relatively low, it is difficult to carry out heat coupling to other rectifying columns, cause the energy unrestrained
Take, in addition to this, above system is increasing with polysilicon plant layout, and single line production capacity is increasing, distillation system tower
The diameter and height of device are also increasing, and the Design cooling load of pump and system increases, and fault in production rate also increases.
Therefore, how to improve the separation of polysilicon cold hydrogenation product and purifying plant, to reduce distillation system load, realize with
Smaller fixation means realize higher efficiency and lower failure rate, become those skilled in the art's weight urgently to be resolved hurrily
Want technical problem.
Invention content
In view of this, first of the present invention is designed to provide a kind of separation of polysilicon cold hydrogenation product and purification dress
It sets, to reduce distillation system load, realizes and to realize higher efficiency and lower failure rate with smaller fixation means, this
Second of invention is designed to provide a kind of polysilicon cold based on the separation of above-mentioned polysilicon cold hydrogenation product and purifying plant
Hydrogenation product detaches and method of purification.
To achieve the above object, the present invention provides the following technical solutions：
A kind of separation of polysilicon cold hydrogenation product and purifying plant, including level-one crude tower and two level crude tower, it is described
Level-one crude tower does not detach STC, and the two level crude tower detaches STC, and the feed(raw material)inlet of the level-one crude tower is cold for receiving
Hydrogenation product, the tower top outlet of the level-one crude tower are connected to the feed(raw material)inlet of the two level crude tower, the two level rough segmentation
The tower top outlet of tower is connected to the distillation system in downstream, and the kettle material of the two level crude tower returns to cold hydrogenation apparatus.
Preferably, it is in series between the tower top outlet of the level-one crude tower and the feed(raw material)inlet of the two level crude tower anti-
Disproportionation reactor or adsorptive reactor.
Preferably, ion exchange resin, absorption resin and suction are housed in the anti-disproportionation reactor or adsorptive reactor
At least one of attached dose.
Preferably, the level-one crude tower tower stripping section is connected by producing the feed(raw material)inlet of device and the cold hydrogenation apparatus
It is logical.
Preferably, further include STC purifying columns, the tower reactor of the feed(raw material)inlet of the STC purifying columns and the level-one crude tower
Outlet, the tower top outlet of the STC purifying columns are connected to the feed(raw material)inlet of the cold hydrogenation apparatus, the STC purifying columns
Tower reactor outlet be connected to STC retracting devices.
Preferably, the feed(raw material)inlet of the STC purifying columns is connected to STC replenishment systems.
Preferably, the tower top entrance of the two level crude tower is for supplementing TCS.
Preferably, the distillation system includes concatenated level-one rectifying column and two-stage rectification tower, the level-one rectifying column
Feed(raw material)inlet be connected to the tower top outlet of the two level crude tower, the outlet of the tower reactor of the level-one rectifying column and two level essence
Evaporate the feed(raw material)inlet connection of tower.
Preferably, the tower reactor of the two-stage rectification tower is provided with the overhead vapours offer heat source of the level-one crude tower
The first coupling reboiler, the overhead vapours that the tower reactor of the level-one rectifying column is provided with the two-stage rectification tower provides heat
The second coupling reboiler in source.
A kind of separation of polysilicon cold hydrogenation product and method of purification, including step：
1) chlorosilane that level-one crude tower generates cold hydrogenation carries out separating-purifying, heavy constituent in cold hydrogenation product and
Part silicon tetrachloride, which enters tower reactor, becomes kettle material, and the other components in cold hydrogenation product enter the tower of level-one crude tower
Top, subsequently into two level crude tower；
2) two level crude tower carries out separating-purifying, silicon tetrachloride and residual weight to the other components in cold hydrogenation product
Component is separated from the tower reactor of two level crude tower and directly returns to cold hydrogenation apparatus as raw material, remaining group lease making two level rough segmentation
The distillation system that the tower top of tower enters downstream continues with.
Preferably, the silicon tetrachloride in the kettle material of the level-one crude tower accounts for whole silicon tetrachlorides in cold hydrogenation product
5%-90%.
Preferably, the tower top material of the tower top material of the level-one crude tower and the two level crude tower is by absorption
Upstream device is entered back into after reaction.
In order to reach above-mentioned first purpose, polysilicon cold hydrogenation product separation provided by the invention and purifying plant, packet
Include level-one crude tower and two level crude tower, wherein level-one crude tower does not detach STC, and two level crude tower detaches STC, and level-one is thick
The feed(raw material)inlet of tower is divided to connect with the feed(raw material)inlet of two level crude tower for receiving cold hydrogenation product, the tower top outlet of level-one crude tower
Logical, the tower top outlet of two level crude tower is connected to the distillation system in downstream, and the kettle material of two level crude tower returns to cold hydrogenation dress
It sets；
Above-mentioned polysilicon cold hydrogenation product separation and purifying plant, rough segmentation system is in series by two-stage crude tower, makes
Used time, level-one crude tower do not detach silicon tetrachloride, in level-one crude tower, a large amount of heavy constituents (high-boiling components) in cold hydrogenation product
And part silicon tetrachloride enters the tower reactor of level-one crude tower, cold hydrogenation overhead extraction silicon tetrachloride realizes removal high-boiling components
Purpose, and remaining trichlorosilane, dichlorosilane and a large amount of silicon tetrachloride be from level-one crude tower overhead extraction, due to tower top
There is a large amount of silicon tetrachloride in extraction component, the saturation temperature of its tower top is caused to be relatively higher than the traditional crude tower of existing system
Tower top temperature, therefore the heat of level-one rough segmentation column overhead is coupled for downstream tower and is used, to save the energy；In two level crude tower
In, silicon tetrachloride and residual heavy constituent are separated from tower reactor, and trichlorosilane and dichlorosilane then enter subsequently from overhead extraction
Rectification process, the silicon tetrachloride of tower reactor extraction can directly return to cold hydrogenation apparatus and directly be used as raw material, without again
The secondary purification by rectifying column；
It can be seen that above-mentioned polysilicon cold hydrogenation product separation and purifying plant use two-stage rough segmentation Deethanizer design, chlorosilane
After the purification that have passed through two-stage crude tower, purity is higher, and the pressure of follow-up rectification process is just very small, slightly light purification,
Product quality accomplishes that 1 grade of solar energy or more rank can be realized easily；Simultaneously as level-one crude tower has detached a part four
Silicon chloride, the silicon tetrachloride into two level crude tower are only a portion in raw material, and percentage amounts are relatively shorter than existing skill
Silicon tetrachloride percentage composition in the charging of art tradition crude tower, therefore the minimum number of theoretical plate of two level crude tower can be less than the prior art
The minimum number of theoretical plate of middle tradition crude tower namely the load and energy consumption of two level crude tower can be relatively low, help to drop
The scale and input of low distillation system, to reduce fault in production rate.
In order to reach above-mentioned second purpose, the present invention also provides a kind of separation of polysilicon cold hydrogenation product and purification sides
Method, this method is based on above-mentioned polysilicon cold hydrogenation product separation and purifying plant, due to above-mentioned polysilicon cold hydrogenation product
Separation and purifying plant have above-mentioned technique effect, the polysilicon cold based on polysilicon cold hydrogenation product separation and purifying plant
Hydrogenation product detaches and method of purification should also have corresponding technique effect.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
Obtain other attached drawings according to these attached drawings.
Fig. 1 is the separation of polysilicon cold hydrogenation product in the prior art and the structural schematic diagram of purifying plant；
Fig. 2 is the structure of rough segmentation system in polysilicon cold hydrogenation product provided in an embodiment of the present invention separation and purifying plant
Schematic diagram；
Fig. 3 is the structural schematic diagram of polysilicon cold hydrogenation product provided in an embodiment of the present invention separation and purifying plant.
In Fig. 2 and Fig. 3：
1 is level-one crude tower；2 be two level crude tower；3 be STC purifying columns；4 be anti-disproportionation reactor or adsorptive reactor；
5 be level-one rectifying column；6 be two-stage rectification tower；7 be adsorptive reactor.
Specific implementation mode
First of the present invention is designed to provide a kind of separation of polysilicon cold hydrogenation product and purifying plant, the polysilicon
Cold hydrogenation product separation and purifying plant can reduce distillation system load, realize higher to realize with smaller fixation means
Efficiency and lower failure rate, second object of the present invention are to provide a kind of based on above-mentioned polysilicon cold hydrogenation product point
From and purifying plant polysilicon cold hydrogenation product separation and method of purification.
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Referring to Fig. 2, Fig. 2 is rough segmentation in polysilicon cold hydrogenation product provided in an embodiment of the present invention separation and purifying plant
The structural schematic diagram of system.
An embodiment of the present invention provides a kind of separation of polysilicon cold hydrogenation product and purifying plant, the rough segmentation systems of the device
It is made of two-stage, including level-one crude tower 1 and two level crude tower 2.
Wherein, level-one crude tower 1 is not used in separation STC (silicon tetrachloride), is mainly used for removing the weight in cold hydrogenation product
Component high-boiling components, two level crude tower 2 detach STC, are mainly used for detaching silicon tetrachloride with trichlorosilane and dichlorosilane, level-one
The feed(raw material)inlet of crude tower 1 for receiving cold hydrogenation product, the feed(raw material)inlet of level-one crude tower 1 can directly with cold hydrogenation apparatus
Products export connection, can also be connected by intermediate storage tank field, the tower top outlet of level-one crude tower 1 and two level crude tower 2
Feed(raw material)inlet connection, the tower top outlet of two level crude tower 2 is connected to the distillation system in downstream, the tower reactor object of two level crude tower 2
Material returns to cold hydrogenation apparatus.
When in use, in level-one crude tower 1, four chlorination of a large amount of heavy constituents (high-boiling components) and part in cold hydrogenation product
Silicon enters the tower reactor of level-one crude tower 1, and cold hydrogenation overhead extraction silicon tetrachloride realizes the purpose of removal high-boiling components, and remaining
Trichlorosilane, dichlorosilane and a large amount of silicon tetrachloride are from 1 overhead extraction of level-one crude tower, due to having in overhead extraction component
A large amount of silicon tetrachloride causes the saturation temperature of its tower top to be relatively higher than the tower top temperature of the traditional crude tower of existing system, therefore
The heat of 1 tower top of level-one crude tower is coupled for downstream tower and is used, to save the energy；In two level crude tower 2, silicon tetrachloride
It is separated from tower reactor with residual heavy constituent, trichlorosilane and dichlorosilane then enter subsequent rectification process from overhead extraction,
The silicon tetrachloride of tower reactor extraction can directly return to cold hydrogenation apparatus and directly be used as raw material, without again passing by rectifying column
Purification.
Compared with prior art, polysilicon cold hydrogenation product separation provided by the invention and purifying plant, by rough segmentation
System carries out two-stage design, and for chlorosilane after the purification of two-stage crude tower, purity is higher, the pressure of follow-up rectification process
Power is just very small, and slightly light purification, product quality accomplishes that 1 grade of solar energy or more rank can be realized easily；Simultaneously as level-one rough segmentation
Tower 1 has detached a part of silicon tetrachloride, and the silicon tetrachloride into two level crude tower 2 is only a portion in raw material,
Its percentage amounts is relatively shorter than the silicon tetrachloride percentage composition in the charging of prior art tradition crude tower, therefore two level crude tower 2 is most
Small number of theoretical plate can be less than traditional minimum number of theoretical plate of crude tower namely the load and energy of two level crude tower 2 in the prior art
Source consumption can be relatively low, contributes to the scale and input that reduce distillation system, to reduce fault in production rate.
Although level-one crude tower 1 removes most heavy constituent high-boiling components, the overhead extraction of level-one crude tower 1
Still contain a certain amount of heavy metal and impurity in object, to improve the refining effect of two level crude tower 2, in the embodiment of the present invention
In, it is in series with anti-disproportionation reactor between the tower top outlet and the feed(raw material)inlet of two level crude tower 2 of level-one crude tower 1 or absorption is anti-
Device 4 is answered, further, equipped with ion exchange resin, absorption resin and adsorbent in anti-disproportionation reactor or adsorptive reactor 4
At least one of, anti-disproportionation reactor or adsorptive reactor 4 can carry out further the overhead extraction object of level-one crude tower 1
Purification, and since crude tower has removed nearly all overweight metal high-boiling components, therefore anti-disproportionation reactor or adsorption reaction
Resin or adsorbent in device 4 not will produce heavy metal poisoning, can not only purify material, can also be used for a long time.While because
Anti- disproportionated reaction can occur without having to worry about material if reactor is anti-disproportionation reactor containing excessive silicon tetrachloride in material
Generate single silane.
Trichlorosilane, silicon tetrachloride and a small amount of dichlorosilane of 1 tower top of level-one crude tower enter two level crude tower 2 and are divided
From silicon tetrachloride and residual heavy constituent are separated from the tower reactor of two level crude tower 2, and trichlorosilane and dichlorosilane are then from two level
The overhead extraction of crude tower 2 enters the distillation system in downstream.Because material have passed through anti-disproportionated reaction before entering two level crude tower 2
The purification of device or adsorptive reactor 4, silicon tetrachloride is more clean, therefore after the separation of two level crude tower 2, and silicon tetrachloride can be with
It directly returns to cold hydrogenation apparatus directly to use as raw material, without again passing by the purification of rectifying column.
Above-mentioned technical proposal is advanced optimized, in embodiments of the present invention, the separation of polysilicon cold hydrogenation product and purification dress
It further includes STC purifying columns 3 to set, the feed(raw material)inlet of STC purifying columns 3 and the tower reactor outlet of level-one crude tower 1, STC purifying columns 3
Tower top outlet be connected to the feed(raw material)inlet of cold hydrogenation apparatus, the outlet of the tower reactors of STC purifying columns 3 is connected to STC retracting devices, one
The kettle material of grade crude tower 1, i.e., the silicon tetrachloride containing heavy constituent impurity are purified in STC purifying columns 3, STC purifications
The material of 3 overhead extraction of tower is the silicon tetrachloride after purification, can directly return to cold hydrogenation apparatus and use, the useless tetrachloro of tower reactor extraction
Change carbon and is then passed through retracting device evaporation or hydrolysis.
Preferably, to improve the refining effect of STC purifying columns 3, in embodiments of the present invention, the raw material of STC purifying columns 3 enters
Mouth is connected to STC replenishment systems, which can be four recycled in the silicon tetrachloride either system additionally supplemented
Silicon chloride.
Further to mitigate the load of above-mentioned STC purifying columns 3, in embodiments of the present invention, as shown in Fig. 2, level-one rough segmentation
1 tower stripping section of tower is connected to by producing device with the feed(raw material)inlet of cold hydrogenation apparatus.
Whether above-mentioned STC purifying columns 3 are arranged depending on specific cold hydrogenation process and other auxiliary facilities, if specific cold
Facility containing similar functions in hydrogenation process or other auxiliary facilities, then this STC purifying column 3 can not design here.
Above-mentioned technical proposal is advanced optimized, the tower top entrance of two level crude tower 2 is mended for supplementing TCS (trichlorosilane)
The TCS filled comes from internal system cycle or additional supplement, to improve the refining effect of two level crude tower 2.
As mentioned above due to the rough segmentation system in the embodiment of the present invention uses two-layer configuration, the distillation system pressure in downstream
It is smaller, therefore, in embodiments of the present invention, referring to Fig. 3, Fig. 3 is polysilicon cold hydrogenation product provided in an embodiment of the present invention
The structural schematic diagram of separation and purifying plant, distillation system also use two-layer configuration, and distillation system includes concatenated level-one essence
Tower 5 and two-stage rectification tower 6 are evaporated, the feed(raw material)inlet of level-one rectifying column 5 is connected to the tower top outlet of two level crude tower 2, level-one essence
The tower reactor outlet for evaporating tower 5 is connected to the feed(raw material)inlet of two-stage rectification tower 6.
When in use, level-one rectifying column 5 removes the overhead extraction object of two level crude tower 2 light, then in two-stage rectification tower 6
After weight, in the overhead extraction trichlorosilane of two-stage rectification tower 6.
Due to containing a large amount of silicon tetrachloride in the overhead extraction object of level-one crude tower 1, level-one crude tower 1 can be improved
Therefore tower top temperature can couple the overhead vapours of level-one crude tower 1 with the tower bottom of tower in downstream, in embodiments of the present invention,
As shown in figure 3, the tower reactor of two-stage rectification tower 6 is provided with the first coupling of the overhead vapours offer heat source of level-one crude tower 1
Reboiler, the second coupling that the tower reactor of level-one rectifying column 5 is provided with the overhead vapours offer heat source of two-stage rectification tower 6 are boiled again
Device.
Above-mentioned technical proposal is advanced optimized, in embodiments of the present invention, tower top outlet and the level-one essence of two level crude tower 2
It evaporates and is in series with adsorptive reactor 7 between the feed(raw material)inlet of tower 5, it is further carried before material enters distillation system
It is pure.
The present invention also provides it is a kind of based on above-mentioned polysilicon cold hydrogenation product separation and purifying plant a kind of polysilicon
Cold hydrogenation product separation and method of purification, including step：
S1：The chlorosilane that level-one crude tower 1 generates cold hydrogenation carries out separating-purifying, the heavy constituent in cold hydrogenation product with
And part silicon tetrachloride enters tower reactor becomes kettle material, the other components in cold hydrogenation product enter level-one crude tower 1
Tower top, subsequently into two level crude tower 2；
In step sl, the silicon tetrachloride in the kettle material of level-one crude tower 1 accounts for all four chlorinations in cold hydrogenation product
The 5%-90% of silicon, and the silicon tetrachloride in the material of the overhead extraction from level-one crude tower 1 accounts for whole four in cold hydrogenation product
The 10%~95% of silicon chloride in this way, improving the tower top temperature of level-one crude tower 1, and can reduce two level crude tower 2
Load.
S2：Two level crude tower 2 carries out separating-purifying, silicon tetrachloride and residual to the other components in cold hydrogenation product
Heavy constituent is separated from the tower reactor of two level crude tower 2 and directly returns to cold hydrogenation apparatus as raw material, remaining group lease making two level
The distillation system that the tower top of crude tower 2 enters downstream continues with.
Above-mentioned technical proposal is advanced optimized, in embodiments of the present invention, the tower top material and two level of level-one crude tower 1
The tower top material of crude tower 2 enters back into upstream device after adsorption reaction.
This programme is described in detail with reference to specific embodiment and Fig. 3.
In 150000 tons/year of polycrystalline silicon producing device, the yield of cold hydrogenation product is 175 tons/hr, and component is as follows
Table：
| Material | SiCl4 | SiHCl3 | SiH2Cl2 | Other |
| Component (wt%) | 0.742 | 0.247 | 0.01 | 0.001 |
Following flow can realize the separation and purification of its product.The raw material of 175 tons/hr passes through level-one crude tower 1, after purification
The tower reactor of level-one crude tower 1 produces the silicon tetrachloride and heavy constituent of 60 tons/hr, the heavy constituents such as almost all of metal chloride from
The tower reactor of level-one crude tower 1 is plucked out of；The tower top of level-one crude tower 1 then produces silicon tetrachloride, the trichlorosilane of about 115 tons/hr
With the mixture of dichlorosilane, contain the silicon tetrachloride of about 70 tons/hr among these.
The material of 115 tons/hr enters adsorptive reactor 7, and remaining heavy metal and impurity are adsorbed, and it is thick to be subsequently introduced two level
Evaporate tower, the trichlorosilane of internal system cycle or supplement also enters the tower, after 3.5 reflux ratio purification 47 tons of overhead extraction/
The trichlorosilane of hr and the mixture of dichlorosilane, tower reactor then produce the silicon tetrachloride of about 70 tons/hr, the tower of two level crude tower 2
The silicon tetrachloride of kettle extraction directly returns to cold hydrogenation apparatus and participates in hydrogenation because more pure.
The product of the overhead extraction of two level crude tower 2 introduces adsorptive reactor 7, and the product after absorption enters level-one rectifying column
5 except light, be subsequently introduced two-stage rectification tower 6 except after weight by the trichlorosilane of 6 44 tons/hr of overhead extraction of two-stage rectification tower.Wherein two
The reboiler of grade 6 tower reactor of rectifying column uses the heat (H1, H2 in Fig. 3) of 1 tower top of level-one crude tower, and level-one rectifying column 5 is again
Boil the heat (H3, H4 in Fig. 3) that device then uses 6 tower top of two-stage rectification tower.
The supplement silicon tetrachloride of the silicon tetrachloride and 3 tons/hr of the 60 tons impure/hr of 1 tower reactor of level-one crude tower extraction
Enter STC purifying columns 3 together, the 62 tons/hr of silicon tetrachloride of 3 overhead extraction of STC purifying columns returns to cold hydrogenation apparatus, tower reactor extraction
The silicon tetrachloride containing high-boiling components of 1 ton/hr then send out and be evaporated or hydrolyze recovery processing.
Whole system only consumes 0.4MPaG steam less than 50 tons/hr, only just corresponds to the cold hydrogenation of traditional improved Siemens
The energy-output ratio of 5 10,000 tons rough segmentation of rectifying+distillation system, but the separation and purification of the cold hydrogenation product of 15 10,000 tons are completed,
And because it have passed through multistage except weight and absorption and adsorbs again, trichlorosilane products can be by the BCl of the 1000ppm in raw material3
And PCl3The boron phosphorus content of 5 overhead extraction of level-one rectifying column is purified in 10-20 or less ranks.
Each embodiment is described by the way of progressive in this specification, the highlights of each of the examples are with other
The difference of embodiment, just to refer each other for identical similar portion between each embodiment.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest range caused.
Claims (12)
1. a kind of polysilicon cold hydrogenation product separation and purifying plant, which is characterized in that thick including level-one crude tower and two level
Tower, the level-one crude tower is divided not to detach STC, the two level crude tower detaches STC, and the feed(raw material)inlet of the level-one crude tower is used
In receiving cold hydrogenation product, the tower top outlet of the level-one crude tower is connected to the feed(raw material)inlet of the two level crude tower, described
The tower top outlet of two level crude tower is connected to the distillation system in downstream, and the kettle material of the two level crude tower returns to cold hydrogenation dress
It sets.
2. polysilicon cold hydrogenation product separation according to claim 1 and purifying plant, which is characterized in that the level-one is thick
It is in series with anti-disproportionation reactor or adsorptive reactor between the tower top outlet and the feed(raw material)inlet of the two level crude tower of point tower.
3. polysilicon cold hydrogenation product separation according to claim 2 and purifying plant, which is characterized in that the anti-disproportionation
Equipped with ion exchange resin, absorption at least one of resin and adsorbent in reactor or adsorptive reactor.
4. the polysilicon cold hydrogenation product separation according to claim 1-3 any one and purifying plant, which is characterized in that
The level-one crude tower tower stripping section is connected to by producing device with the feed(raw material)inlet of the cold hydrogenation apparatus.
5. the polysilicon cold hydrogenation product separation according to claim 1-3 any one and purifying plant, which is characterized in that
Further include STC purifying columns, the tower reactor outlet of the feed(raw material)inlet of the STC purifying columns and the level-one crude tower, the STC
The tower top outlet of purifying column is connected to the feed(raw material)inlet of the cold hydrogenation apparatus, and tower reactor outlet and the STC of the STC purifying columns are returned
Receiving apparatus is connected to.
6. polysilicon cold hydrogenation product separation according to claim 5 and purifying plant, which is characterized in that the STC is carried
The feed(raw material)inlet of pure tower is connected to STC replenishment systems.
7. the separation of polysilicon cold hydrogenation product and purifying plant, feature according to claim 1-3 and 6 any one exist
In the tower top entrance of the two level crude tower is for supplementing TCS.
8. the separation of polysilicon cold hydrogenation product and purifying plant, feature according to claim 1-3 and 6 any one exist
In, the distillation system include concatenated level-one rectifying column and two-stage rectification tower, the feed(raw material)inlet of the level-one rectifying column with
The tower top outlet of the two level crude tower is connected to, and the tower reactor outlet of the level-one rectifying column and the raw material of the two-stage rectification tower enter
Mouth connection.
9. polysilicon cold hydrogenation product separation according to claim 8 and purifying plant, which is characterized in that the two level essence
Evaporate tower tower reactor be provided with the level-one crude tower overhead vapours provide heat source first coupling reboiler, the level-one
The tower reactor of rectifying column is provided with the second coupling reboiler of the overhead vapours offer heat source of the two-stage rectification tower.
10. a kind of polysilicon cold hydrogenation product separation and method of purification, which is characterized in that including step：
1) chlorosilane that level-one crude tower generates cold hydrogenation carries out separating-purifying, the heavy constituent in cold hydrogenation product and part
Silicon tetrachloride, which enters tower reactor, becomes kettle material, and the other components in cold hydrogenation product enter the tower top of level-one crude tower,
Subsequently into two level crude tower；
2) two level crude tower carries out separating-purifying, silicon tetrachloride and residual heavy constituent to the other components in cold hydrogenation product
It is separated from the tower reactor of two level crude tower and directly returns to cold hydrogenation apparatus as raw material, remaining organizes lease making two level crude tower
The distillation system that tower top enters downstream continues with.
11. polysilicon cold hydrogenation product separation according to claim 10 and purifying plant, which is characterized in that the level-one
Silicon tetrachloride in the kettle material of crude tower accounts for the 5%-90% of whole silicon tetrachlorides in cold hydrogenation product.
12. polysilicon cold hydrogenation product separation according to claim 10 and purifying plant, which is characterized in that the level-one
The tower top material of the tower top material of crude tower and the two level crude tower enters back into upstream device after adsorption reaction.
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