CN104071791B - The method of purification of trichlorosilane - Google Patents
The method of purification of trichlorosilane Download PDFInfo
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- CN104071791B CN104071791B CN201410331701.3A CN201410331701A CN104071791B CN 104071791 B CN104071791 B CN 104071791B CN 201410331701 A CN201410331701 A CN 201410331701A CN 104071791 B CN104071791 B CN 104071791B
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Abstract
The invention discloses the method for purification of a kind of trichlorosilane.The method includes thick for trichlorosilane liquid is passed through the step purifying tower system, the step that thick for trichlorosilane liquid is passed through purification tower system includes: is passed through by thick for trichlorosilane liquid and includes that the weight-removing column group of at least two weight-removing column carries out taking off heavily processing successively, heavily processes, through de-, the low-boiling-point substance obtained to obtain；To include that the lightness-removing column group of at least one lightness-removing column carries out de-gently process, to obtain trichlorosilane successively through the de-low-boiling-point substance feeding obtained that heavily processes.In the method, thick for trichlorosilane liquid is first passed through weight-removing column group again by lightness-removing column group, thick liquid can be made to carry out de-light industry sequence again after carrying out de-heavy industry sequence.This leading portion de-weight continuously, back segment take off light arranging continuously and can the silicon powder impurity in thick liquid, high boiling point chloride and high boiling point metallic chloride impurities be separated during the de-weight of leading portion, thus the impurity that these easily cause blocking concentrates in leading portion weight-removing column, reduce subsequent purification tower and the blocking probability of reboiler.
Description
Technical field
The present invention relates to polysilicon and manufacture field, in particular to the method for purification of a kind of trichlorosilane.
Background technology
Polysilicon is to manufacture semiconductor device, integrated circuit, the basic material of solar cell material, is information and energy industry
Foundation stone, be also that country encourages the strategic material first developed.The most most polysilicon passes through improved Siemens at present
Prepare.This method mainly includes trichlorosilane synthesis, rectification and purification, reduction, tail gas recycle and hydrogenation five processes.Wherein, essence
Evaporate purification process and be to ensure that the important procedure of polysilicon purity.
In existing rectification and purification operation, it is that thick for trichlorosilane liquid is purified by purifying tower system.But, at trichlorosilane
During the building-up process of thick liquid and hydrogenation of silicon tetrachloride, needing using thick silica flour as raw material, this allows in the thick liquid of trichlorosilane
Containing more unreacted silica flour and some other high boiling point metallic compound.During the rectification and purification in later stage, by three
When the thick liquid of chlorine hydrogen silicon carries out condensation repeatedly and vaporization, these silica flours and metallic compound are easy at phase transformation gather.With
Time, these materials are also easy at the bottom of tower, gather in reboiler and pipeline thereof.Ultimately result in tower reactor and reboiler Severe blockage,
Reduce the heat transfer effect of reboiler, even cause whole tower system parking maintenance.This greatly reduces the system stability of tower system, more
Have a strong impact on the seriality of production of polysilicon.
For these reasons, it is necessary to propose a kind of new method of purification, in order to alleviate in rectification and purification operation purify tower system easily block up
The problem of plug.
Summary of the invention
It is desirable to provide the method for purification of a kind of trichlorosilane, easy to solve purification tower system in prior art rectification and purification operation
The problem of blocking.
To achieve these goals, according to an aspect of the invention, it is provided the method for purification of a kind of trichlorosilane, it includes
Thick for trichlorosilane liquid is passed through the step purifying tower system, and this step that thick for trichlorosilane liquid is passed through purification tower system includes: by trichlorine
The thick liquid of hydrogen silicon is passed through and includes that the weight-removing column group of at least two weight-removing column carries out de-heavily process, to obtain through taking off what heavily process obtained successively
Low-boiling-point substance；To include that the lightness-removing column group of at least one lightness-removing column carries out taking off light process successively through the de-low-boiling-point substance feeding obtained that heavily processes,
To obtain trichlorosilane.
Further, weight-removing column group includes that at least two weight-removing column, lightness-removing column group include at least two lightness-removing column, and weight-removing column with
The sum of lightness-removing column is four to six.
Further, before thick for trichlorosilane liquid is passed through the step purifying tower system, also include thick for trichlorosilane liquid is being stood reservoir
Standing sedimentation in tank, obtains the step of upper liquid；After the step of standing sedimentation, upper liquid is passed through purification tower system.
Further, in the step of standing sedimentation, time of repose is 5～60min, preferably 10～20min.
Further, before upper liquid is passed through the step of described purification tower system, also include that upper liquid is passed through defecator to be carried out
Filter, obtains the step of filtrate；After filtration step, filtrate is passed through purification tower system.
Further, in the step of filtration, in filtrate, grain diameter is less than 100 mesh.
Further, the reboiler that tower system includes arranging is purified with each weight-removing column and each lightness-removing column one_to_one corresponding.
Further, each reboiler is forced cyclic type reboiler or thermosiphon reboiler.
Further, being passed through by thick for trichlorosilane liquid in the step purifying tower system, the flow velocity controlling to flow into the liquid of each reboiler is
5～6m/s.
Further, thick for trichlorosilane liquid is passed through in the step purifying tower system, uses different recycling cans to be separately recovered each de-weight
The high-boiling components that tower produces, and the low-boiling-point substance that each lightness-removing column produces.
The method of purification of a kind of trichlorosilane of the application present invention, first passes through weight-removing column group by thick for trichlorosilane liquid, then by de-light
Tower system, can make the thick liquid of trichlorosilane carry out de-light industry sequence after carrying out de-heavy industry sequence again.This leading portion de-weight, back segment continuously
The most de-light being provided with beneficially by the silicon powder impurity in thick for trichlorosilane liquid, high boiling point chloride and high boiling point metal chloride
Impurity is separated during the de-weight of leading portion, thus the impurity that these easily cause tower system blocking concentrates on the de-weight of leading portion
In tower (the especially first weight-removing column), reduce subsequent purification tower and the blocking probability of reboiler.
Accompanying drawing explanation
The Figure of description of the part constituting the application is used for providing a further understanding of the present invention, and the present invention's is schematic real
Execute example and illustrate for explaining the present invention, being not intended that inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 shows according to the purifying plant schematic diagram used in the method for purification of the trichlorosilane of one embodiment of the present invention.
Detailed description of the invention
It should be noted that in the case of not conflicting, the embodiment in the application and the feature in embodiment can be mutually combined.
The present invention is described in detail below in conjunction with embodiment.
As background section is introduced, there is susceptible to plugging problem in the purification tower system of existing trichlorosilane.In order to solve
This problem, inventor provides the method for purification of a kind of trichlorosilane, and it includes thick for trichlorosilane liquid is passed through purification
The step of tower system, this step that thick for trichlorosilane liquid is passed through purification tower system includes: is passed through by thick for trichlorosilane liquid and includes at least two
The weight-removing column group of individual weight-removing column carries out taking off heavily processing successively, heavily processes, through de-, the low-boiling-point substance obtained to obtain；Heavily will process through de-
To low-boiling-point substance send into and include that the lightness-removing column group of at least one lightness-removing column carries out de-light process, to obtain trichlorosilane successively.
The method of purification of the trichlorosilane that the present invention is above-mentioned can be by by the purification by following trichlorosilane of thick for the trichlorosilane liquid
Device realizes.Specifically, this purifying plant includes purifying tower system, wherein, as it is shown in figure 1, purify tower system to include weight-removing column
Group 100 and lightness-removing column group 200, weight-removing column group 100 includes that at least two weight-removing column 110, lightness-removing column group 200 include at least one
Lightness-removing column 210；According to Flow of Goods and Materials order, weight-removing column group 100 is arranged on the upstream of lightness-removing column group 200.
In above-mentioned method of purification provided by the present invention, thick for trichlorosilane liquid is first passed through weight-removing column group, then by lightness-removing column group,
The thick liquid of trichlorosilane can be made to carry out de-light industry sequence after carrying out de-heavy industry sequence again.This leading portion de-weight, back segment continuously take off continuously
Silicon powder impurity in thick for trichlorosilane liquid, high boiling point chloride and high boiling point metallic chloride impurities are beneficially existed by light being provided with
It is separated during the de-weight of leading portion, thus the impurity that these easily cause tower system blocking concentrates on the weight-removing column 110 of leading portion
In especially first weight-removing column 110, reduce subsequent purification tower and the blocking probability of reboiler 101.
During practical operation, as long as thick for trichlorosilane liquid to be first passed through weight-removing column group, then by lightness-removing column group, the most favourable
In the solid particle in thick for trichlorosilane liquid, high-boiling-point impurity are concentrated in leading portion weight-removing column 110.Concrete weight-removing column 110
Can be adjusted according to the composition of the concrete thick liquid of trichlorosilane with the number of lightness-removing column 210.In one preferred embodiment
In, weight-removing column group 100 includes that at least two weight-removing column 110, lightness-removing column group 200 include at least two lightness-removing column 210, and de-weight
Tower 110 is four to six with the sum of lightness-removing column 210.
In above-mentioned method of purification, thick for trichlorosilane liquid is carried out the most de-weight by weight-removing column group 100, it becomes possible to by major part
Solid granulates, high-boiling-point impurity carry out concentrating separation.In a preferred embodiment, thick for trichlorosilane liquid is passed through purification
Before the step of tower system, also include, by thick for trichlorosilane liquid standing sedimentation in standing receiver, obtaining the step of upper liquid；Quiet
After putting the step of sedimentation, upper liquid is passed through purification tower system.Through standing in receiver, be conducive to removing in thick liquid the most anti-
Should solid granulates completely, thus advantageously reduce the blocking probability of follow-up tower system.During practical operation, standing sedimentation
Step in time of repose can be adjusted according to the granule content in thick liquid.For the consideration of production efficiency, preferably this standing
Time is 5～60min, more preferably 10～20min.By thick liquid after standing processes, most of unreacted solid granulates are equal
Can be removed.In a kind of preferred embodiment, before upper liquid is passed through the step purifying tower system, also include upper liquid
It is passed through 400 to filter, obtains the step of filtrate；After filtration step, filtrate is passed through purification tower system.The step preferably filtered
In Zhou, in filtrate, grain diameter is less than 100 mesh.Above-mentioned filtration step is conducive to the molecule further filtering out in upper liquid,
Thus reduce the blocking probability of follow-up tower system further.
Correspondingly, above-mentioned thick for trichlorosilane liquid is being stood in receiver standing sedimentation and passed through by standing receiver liquid at the middle and upper levels
The step of filter device can be realized by following device.Specifically, as it is shown in figure 1, above-mentioned purifying plant also includes according to material
Sequence of flow is arranged on the standing receiver 300 of weight-removing column group 100 upstream, stands upper liquid outlet and the purifying column of receiver 300
The charging aperture of group is connected.Before the thick liquid of trichlorosilane enters weight-removing column group 100, first thick liquid is passed through standing receiver 300, has
It is beneficial to make the solid granulates that in thick liquid, major part unreacted is complete sink to bottom receiver.Thus the blocking that reduces follow-up weight-removing column 110 is several
Rate, improves the seriality of Trichlorosilane purification operation.It is highly preferred that above-mentioned purifying plant also includes being arranged on standing receiver 300
Upper liquid outlet with purify tower system charging aperture between defecator 400, defecator 400 is used for filtering particle diameter in upper liquid
Granule more than or equal to 100 mesh.The upper liquid stood in receiver 300 is passed through defecator 400, it is possible to remove thick further
Solid granulates in liquid, thus reduce the blocking probability of follow-up weight-removing column 110 further, improve the continuous of Trichlorosilane purification operation
Property.
In above-mentioned purification tower system, the heating of reboiler is generally utilized to realize the vaporization of material.In a preferred embodiment,
Above-mentioned purification tower system includes the reboiler 101 arranged with each weight-removing column 110 and each lightness-removing column 210 one_to_one corresponding, it is preferable that each
Reboiler 101 is forced cyclic type reboiler 101 or thermosiphon reboiler 101, more preferably forced cyclic type reboiler 101.
Flow rate of liquid in forced circulating reboiler 101 is very fast.Scale velocity during flow rate of liquid advantageously reduces pipeline faster, with
Time, the liquid of high flow rate can also play the effect washing away pipeline inner wall.Thus be conducive to alleviating further reboiler 101 pipeline
Blockage problem.In practical operation, on the premise of meeting thermal transmission requirement, preferably thick for trichlorosilane liquid is being passed through purifying column
In the step of group, the flow rate of liquid controlling to flow into each reboiler 101 is 5～6m/s.Use the reboiler 101 of above-mentioned higher range
Flow rate of liquid, advantageously reduces the scale velocity in pipeline, and meanwhile, the liquid of high flow rate can also play and wash away pipeline inner wall
Effect.Thus be conducive to alleviating further the blockage problem of reboiler 101 pipeline.It addition, high flow rate can improve reboiler 101
The coefficient of heat transfer, improve reboiler 101 heat transfer effect such that it is able on the basis of the reboiler 101 slight fouling of pipeline,
It is made to remain on higher heat transfer effect.The concrete method of flow rate of liquid in reboiler 101 that adjusts can be art technology
Personnel's customary way, it is preferable that by solid circulating rate in reduction reboiler 101 vaporization rate raising reboiler 101, or
Being accelerated by pump pressurization, in making reboiler 101, material flow reaches 5～6m/s
During reclaiming residual liquid, it is preferred to use different recycling cans 102 is separately recovered the high-boiling components that each weight-removing column 110 produces,
And each lightness-removing column 210 produces low-boiling-point substance.It is separately recovered residual liquid in tower to be conducive to the high-boiling components in thick for trichlorosilane liquid and low boiling
Thing carries out post processing and recycling respectively.Specifically, above-mentioned purification tower system also includes the tower reactor outlet with each weight-removing column 110, with
And the recycling can 102 that the tower top outlet one_to_one corresponding of each lightness-removing column 210 is arranged.
In the above-mentioned method of purification that the present invention provides, after thick for trichlorosilane liquid is carried out the most de-weight, then carry out de-light industry sequence.This
Plant method of purification to be conducive to the silicon powder impurity in thick for trichlorosilane liquid, high boiling point chloride and high boiling point metallic chloride impurities
It is separated during the de-weight of leading portion, thus the impurity that these easily cause tower system blocking concentrates in the weight-removing column of leading portion,
Reduce subsequent purification tower and the blocking probability of reboiler.By in time the high-boiling components residual liquid in weight-removing column tower reactor being discharged, just
The probability that whole purification tower system is blocked can be reduced, improve the operation seriality purifying tower system.
Being described in further detail the present invention below in conjunction with specific embodiment, these embodiments are it is not intended that limit institute of the present invention
Claimed scope.
Embodiment 1
Purification tower system liquid thick to trichlorosilane is used to purify.Wherein, purify tower system and include weight-removing column group and lightness-removing column group, de-
Weight tower system is arranged on lightness-removing column group upstream, and weight-removing column group includes that the first weight-removing column, the second weight-removing column and the 3rd that are sequentially connected are de-
Weight tower, lightness-removing column group includes the first lightness-removing column and the second lightness-removing column being sequentially connected, and each tower is furnished with forced cyclic type reboiler, then
Flow rate of liquid in boiling device is 3m/s.
After running 180d continuously, there is blocking in the first weight-removing column pipeline.
Embodiment 2
After thick for trichlorosilane liquid is stood 10min by standing receiver, upper liquid is passed through purification tower system and purifies.Wherein,
Purifying tower system and include weight-removing column group and lightness-removing column group, weight-removing column group is arranged on lightness-removing column group upstream, and weight-removing column group includes phase successively
The first weight-removing column, the second weight-removing column and the 3rd weight-removing column even, lightness-removing column group includes that the first lightness-removing column being sequentially connected and second takes off
Light tower, each tower is furnished with forced cyclic type reboiler.Flow rate of liquid in reboiler is 5m/s.
After running 210d continuously, there is blocking in the first weight-removing column pipeline.
Embodiment 3
Thick for trichlorosilane liquid is stood after 10min by standing receiver, upper liquid is passed through defecator and carries out filtration and make filtrate
Middle grain diameter is less than 100 mesh, filtrate is then passed through purification tower system and purifies.Wherein, purify tower system and include weight-removing column group
With lightness-removing column group, weight-removing column group is arranged on lightness-removing column group upstream, and weight-removing column group include being sequentially connected the first weight-removing column, second
Weight-removing column and the 3rd weight-removing column, lightness-removing column group includes the first lightness-removing column and the second lightness-removing column being sequentially connected, and each tower is furnished with pressure and follows
Ring type reboiler.Flow rate of liquid in reboiler is 6m/s.
After running 240d continuously, there is blocking in the first weight-removing column pipeline.
Comparative example 1
Purification tower system liquid thick to trichlorosilane is used to purify.Wherein, purify the first weight-removing column that tower system includes being sequentially connected,
First lightness-removing column, the second weight-removing column, the second lightness-removing column and the 3rd weight-removing column, each tower is furnished with thermosiphon reboiler.In reboiler
Flow rate of liquid is 2m/s.
After running 120d continuously, each weight-removing column, lightness-removing column and reboiler pipeline all occur blocking.
From above data with describe, it can be seen that the purifying method of trichlorosilane of the present invention achieves following technique effect:
1), de-light continuously by thick for trichlorosilane liquid being carried out leading portion de-weight, back segment continuously, be conducive to thick liquid to easily cause tower
The solid granulates of group blocking and high-boiling-point impurity concentrate in the weight-removing column of leading portion, coordinate weight-removing column bottom product timely to reclaim,
The seriality can effectively reduce the blocking probability purifying tower system, improving purification process；
2), by thick for trichlorosilane liquid is carried out into the pretreatment before tower, it is possible to major part solid granulates in thick liquid is removed, enters
One step reduces the blocking probability of follow-up tower system；
3), by improving the flow rate of liquid of reboiler in each weight-removing column and lightness-removing column, the blocking of reboiler pipeline is advantageously reduced
Probability.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for those skilled in the art
For, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, any amendment of being made, etc.
With replacement, improvement etc., should be included within the scope of the present invention.
Claims (9)
1. the method for purification of a trichlorosilane, it is characterised in that include thick for trichlorosilane liquid is passed through the step purifying tower system, institute
State thick for trichlorosilane liquid is passed through purify tower system step include:
Thick for trichlorosilane liquid is passed through and includes that the weight-removing column group of at least two weight-removing column carries out de-heavily process, to obtain warp successively
Take off and heavily process the low-boiling-point substance obtained；
De-for the described warp low-boiling-point substance feeding obtained that heavily processes is included that the lightness-removing column group of at least one lightness-removing column carries out taking off gently successively
Process, to obtain trichlorosilane；
Described purification tower system includes the reboiler arranged with each described weight-removing column and each described lightness-removing column one_to_one corresponding；
Being passed through by thick for trichlorosilane liquid in the step purifying tower system, the flow velocity controlling to flow into the liquid of each reboiler is 5～6m/s.
Method of purification the most according to claim 1, it is characterised in that described weight-removing column group includes at least two weight-removing column, institute
State lightness-removing column group and include at least two lightness-removing column, and the sum of described weight-removing column and described lightness-removing column is four to six.
Method of purification the most according to claim 1, it is characterised in that thick for described trichlorosilane liquid is passed through the step purifying tower system
Before Zhou, also include, by thick for described trichlorosilane liquid standing sedimentation in standing receiver, obtaining the step of upper liquid；Institute
After stating the step of standing sedimentation, described upper liquid is passed through described purification tower system.
Method of purification the most according to claim 3, it is characterised in that in the step of described standing sedimentation, time of repose is
5～60min.
Method of purification the most according to claim 4, it is characterised in that in the step of described standing sedimentation, time of repose is
10～20min.
Method of purification the most according to claim 3, it is characterised in that before described upper liquid is passed through the step of described purification tower system,
Also include that described upper liquid is passed through defecator filters, obtain the step of filtrate；After described filtration step, will
Described filtrate is passed through described purification tower system.
Method of purification the most according to claim 6, it is characterised in that in the step of described filtration, the grain diameter in filtrate is little
In 100 mesh.
Method of purification the most according to claim 1, it is characterised in that each described reboiler is forced cyclic type reboiler or heat
Siphon reboiler.
Method of purification the most according to claim 1, it is characterised in that thick for trichlorosilane liquid is passed through in the step purifying tower system,
Different recycling cans is used to be separately recovered the high-boiling components that each described weight-removing column produces, and the low boiling that each described lightness-removing column produces
Thing.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107055549A (en) * | 2017-04-06 | 2017-08-18 | 洛阳中硅高科技有限公司 | A kind of method for preparing electron level trichlorosilane |
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| CN101538044A (en) * | 2009-04-21 | 2009-09-23 | 天津大学 | System for separating and purifying trichlorosilane in production process of polysilicon and operation method thereof |
| CN102153092A (en) * | 2011-04-27 | 2011-08-17 | 天津大学 | Heat pump distillation and multi-effect distillation integrated device and process for purifying trichlorosilane |
| CN203048612U (en) * | 2013-01-15 | 2013-07-10 | 昆明理工大学 | Trichlorosilane purifying device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538044A (en) * | 2009-04-21 | 2009-09-23 | 天津大学 | System for separating and purifying trichlorosilane in production process of polysilicon and operation method thereof |
| CN102153092A (en) * | 2011-04-27 | 2011-08-17 | 天津大学 | Heat pump distillation and multi-effect distillation integrated device and process for purifying trichlorosilane |
| CN203048612U (en) * | 2013-01-15 | 2013-07-10 | 昆明理工大学 | Trichlorosilane purifying device |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107055549A (en) * | 2017-04-06 | 2017-08-18 | 洛阳中硅高科技有限公司 | A kind of method for preparing electron level trichlorosilane |
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