CN105480981B - The recovery method and device of a kind of dichlorosilane in tail gas in polycrystalline reduction production - Google Patents
The recovery method and device of a kind of dichlorosilane in tail gas in polycrystalline reduction production Download PDFInfo
- Publication number
- CN105480981B CN105480981B CN201410484800.5A CN201410484800A CN105480981B CN 105480981 B CN105480981 B CN 105480981B CN 201410484800 A CN201410484800 A CN 201410484800A CN 105480981 B CN105480981 B CN 105480981B
- Authority
- CN
- China
- Prior art keywords
- dichlorosilane
- tail gas
- tower
- polycrystalline reduction
- chlorosilane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention discloses the recovery method and device of the dichlorosilane in the tail gas in a kind of production of polycrystalline reduction, this method comprises the following steps：(1) tail gas during polycrystalline reduction is produced carries out parsing separation, the hydrogen chloride and chlorosilane separated；(2) absorption is carried out to the chlorosilane and removes the impurity containing boron phosphorus；(3) one-level rectifying removing light component is carried out；(4) two-stage rectification removing heavy constituent is carried out, dichlorosilane is obtained.Substantial amounts of alkali lye and water need not be consumed, dichlorosilane can just be obtained by parsing, absorption, one-level rectifying, two-stage rectification process, vent gas treatment cost is low, pollution is few.
Description
Technical field
The invention belongs to technical field of polysilicon production, and in particular to two in tail gas in a kind of polycrystalline reduction production
The recovery method and device of chlorine dihydro silicon.
Background technology
Polysilicon enterprise can produce substantial amounts of tail gas, the mass rate of emission average out to 5000 of tail gas in polycrystalline reduction production
~10000NM3/h.The main component of above-mentioned tail gas includes：Silicon tetrachloride, trichlorosilane, dichlorosilane, hydrogen chloride, hydrogen
With micro phosphorus trichloride, phosphorus pentachloride, boron chloride, borine, phosphine and metal chloride (wherein, phosphorus trichloride, phosphoric
Phosphorus, boron chloride, borine, phosphine and metal chloride are micro) etc..Under normal circumstances, these tail gas can be all sent to
Raffinate device, is eluted using alkali lye to tail gas, then by being discharged into air after washing.Chlorosilane gas major part in tail gas exists
It is neutralized under alkali lye elution state, the material after neutralization is fed to filter press press filtration and obtains waste residue, waste residue delivers to extraneous progress
Processing.And a large amount of alkali lye and water are consumed during above-mentioned vent gas treatment, vent gas treatment cost is higher.
The content of the invention
The technical problems to be solved by the invention are that there is provided a kind of polysilicon for above shortcomings in the prior art
The recovery method and device of the dichlorosilane in tail gas also in original production, this method processing procedure are simple, without using alkali lye
And water, it can effectively obtain dichlorosilane.
The technical scheme that solution present invention problem is used is to provide in the tail gas in a kind of polycrystalline reduction production
Dichlorosilane recovery method, comprise the following steps：
(1) tail gas during polycrystalline reduction is produced carries out parsing separation, the hydrogen chloride and chlorosilane separated；
(2) absorption is carried out to the chlorosilane and removes the impurity containing boron phosphorus；
(3) one-level rectifying removing light component is carried out；
(4) two-stage rectification removing heavy constituent is carried out, dichlorosilane is obtained.
Preferably, in the step (1), the temperature of the parsing is -50~160 DEG C, and the pressure of the parsing is 0.5
~1.2MPa.
Preferably, in the step (1), the temperature for parsing the chlorosilane separated is -30~-10 DEG C.
Preferably, in the step (2), the composition of the adsorbent used when being adsorbed includes：20%~
The silica gel of 60% mass percent, the aluminum oxide of 10%~30% mass percent and 10%~70% mass percent
Activated carbon.
Preferably, in the step (3), the pressure for carrying out one-level rectifying is 0.4~0.5MPa.
Preferably, in the step (4), the pressure for carrying out two-stage rectification is 0.4~0.5MPa.
The present invention provides the retracting device of the dichlorosilane in the tail gas in a kind of polycrystalline reduction production, including：
Analytic Tower, for polycrystalline reduction to be produced in tail gas carry out parsing separation, the hydrogen chloride separated and
Chlorosilane；
Adsorption column, is connected with the Analytic Tower, and the adsorption column is used to remove containing boron chlorosilane progress absorption
The impurity of phosphorus；
One-level rectifying column, is connected with the adsorption column, and the one-level rectifying column is used to carry out one-level rectifying removing light component；
Two-stage rectification tower, is connected with the one-level rectifying column, and the two-stage rectification tower is used to carry out two-stage rectification removing weight
Component, obtains dichlorosilane.
Preferably, temperature when being parsed in the Analytic Tower is -50~160 DEG C, and pressure is 0.5~1.2MPa
Preferably, the temperature of the tower top of the Analytic Tower is -30~-10 DEG C.
Preferably, the composition of the adsorbent in the adsorption column includes：The silica gel of 20%~60% mass percent,
The activated carbon of the aluminum oxide of 10%~30% mass percent and 10%~70% mass percent.
Preferably, the pressure when one-level rectifying column carries out rectifying is 0.4~0.5MPa.
Preferably, the pressure when two-stage rectification tower carries out rectifying is 0.4~0.5MPa.
Preferably, the one-level rectifying column, the two-stage rectification tower are non-metallic fillers tower, and are liner polytetrafluoro
Ethene packed tower.
The recovery method and device of the dichlorosilane in tail gas in being produced by the polycrystalline reduction in the present invention, no
Need to consume substantial amounts of alkali lye and water, dichloro-dihydro can just be obtained by parsing, absorption, one-level rectifying, two-stage rectification process
Silicon, vent gas treatment cost is low, and pollution is few.
Brief description of the drawings
Fig. 1 is the structural representation of the retracting device of the dichlorosilane in the crystal silicon reduction tail gas in the embodiment of the present invention 2
Figure.
In figure：1- Analytic Towers；The tower top of 11- Analytic Towers；The tower reactor of 12- Analytic Towers；2- adsorption columns；21- adsorption columns enter
Material mouth；The discharging opening of 22- adsorption columns；3- one-level rectifying columns；The charging aperture of 31- one-level rectifying columns；The tower of 32- one-level rectifying columns
Top；The tower reactor of 33- one-level rectifying columns；4- two-stage rectification towers；The charging aperture of 41- two-stage rectification towers；The tower of 42- two-stage rectification towers
Top；The tower reactor of 43- two-stage rectification towers；5- refining trichlorosilane storage tanks.
Embodiment
To make those skilled in the art more fully understand technical scheme, below in conjunction with the accompanying drawings and specific embodiment party
Formula is described in further detail to the present invention.
Embodiment 1
The recovery method of the dichlorosilane in tail gas in a kind of polycrystalline reduction production of the present embodiment offer, including with
Lower step：
(1) tail gas during polycrystalline reduction is produced carries out parsing separation, the hydrogen chloride and chlorosilane separated；
(2) absorption is carried out to the chlorosilane and removes the impurity containing boron phosphorus；
(3) one-level rectifying removing light component is carried out；
(4) two-stage rectification removing heavy constituent is carried out, dichlorosilane is obtained.
Preferably, in the step (1), the temperature of the parsing is -50~160 DEG C, and the pressure of the parsing is 0.5
~1.2MPa.
Preferably, in the step (1), the temperature for parsing the chlorosilane separated is -30~-10 DEG C.
Preferably, in the step (2), the composition of the adsorbent used when being adsorbed includes：20%~
The silica gel of 60% mass percent, the aluminum oxide of 10%~30% mass percent and 10%~70% mass percent
Activated carbon.
Preferably, in the step (3), the pressure for carrying out one-level rectifying is 0.4~0.5MPa.
Preferably, in the step (4), the pressure for carrying out two-stage rectification is 0.4~0.5MPa.
Pass through the recovery method of the dichlorosilane in the tail gas in the polycrystalline reduction production in the present embodiment, it is not necessary to
Substantial amounts of alkali lye and water are consumed, dichlorosilane, tail can just be obtained by parsing, absorption, one-level rectifying, two-stage rectification process
Gas disposal cost is low, and pollution is few.
Embodiment 2
As shown in figure 1, the present embodiment provides the recovery of the dichlorosilane in the tail gas in a kind of polycrystalline reduction production
Device, including：
Analytic Tower 1, for polycrystalline reduction to be produced in tail gas carry out parsing separation, the hydrogen chloride separated and
Chlorosilane.The Analytic Tower 1 is specially hydrogen chloride rich solution knockout tower, and the hydrogen chloride being dissolved in chlorosilane is separated.Can
To carry out pre-separation to chlorosilane by Analytic Tower 1, the produce load of downstream purification separator is reduced.
Tail gas in polycrystalline reduction production mainly includes silicon tetrachloride, trichlorosilane, dichlorosilane, hydrogen chloride, hydrogen
Gas and micro phosphorus trichloride, phosphorus pentachloride, boron chloride, borine, phosphine and metal chloride (wherein, phosphorus trichloride, pentachloro-
It is micro to change phosphorus, boron chloride, borine, phosphine and metal chloride).The boiling point of hydrogen chloride is relatively low (to boil under atmospheric pressure state
Point is -85 DEG C), its boiling-point difference with chlorosilane is away from big, it is possible to pass through the progress parsing separation of Analytic Tower 1.By polysilicon also
Tail gas in original production is carried out after parsing separation by Analytic Tower 1, usual hydrogen chloride analytically tower of tower in the form of fixed gas
Separation is arranged outside the heat exchanger on top 11；Meanwhile, it (is mainly dichloro-dihydro that the tower top 11 of Analytic Tower, which is enriched with more light component chlorosilane,
Silicon and trichlorosilane), the light component chlorosilane of the tower top 11 of Analytic Tower is condensed into liquid phase state, and light component chlorosilane passes through solution
The liquid-phase reflux pipeline for analysing the tower top 11 of tower returns to foundation circulation in Analytic Tower 1；The analytically liquid-phase reflux pipe of the tower top 11 of tower
Line draws the light component chlorosilane of tributary stock extraction liquid phase state, and the tower reactor 12 of Analytic Tower is heavy constituent chlorosilane enrichment region
Domain, heavy constituent chlorosilane analytically tower tower reactor 12 produce after enter downstream purification separator.The light component chlorine of liquid phase state
Mainly include the mixture of trichlorosilane, dichlorosilane and a small amount of hydrogen chloride in silane.
The preliminary pre-separation for completing the tail gas in polycrystalline reduction production, constant in chlorosilane total amount in Analytic Tower 1
In the case of, liquid phase low temperature light component chlorosilane is produced by the tower top 11 of Analytic Tower, the extraction of tower reactor 12 of Analytic Tower is reduced
Heavy constituent chlorosilane enters the chlorosilane amount of downstream purification separator, alleviates the removal of impurities segregational load of downstream purification device,
Especially under production oepration at full load state, the step is particularly important.
Adsorption column 2, is connected with the Analytic Tower 1, the adsorption column 2 be used for the chlorosilane carry out absorption remove containing
The impurity of boron phosphorus.Specifically, the charging aperture 21 of adsorption column is connected with the tower top 11 of Analytic Tower.After adsorption column 2, passed through
The light component chlorosilane crossed after adsorption-edulcoration.Specifically, the adsorption column 2 in the present embodiment is net for the chlorosilane for being filled with adsorbent
Change equipment, the equipment can be by the trace B phosphorus impurities adsorbing and removing in liquid-phase chlorosilane.
One-level rectifying column 3, is connected with the adsorption column 2, and the one-level rectifying column 3 is used to carry out light group of one-level rectifying removing
Point.Specifically, the charging aperture 31 of one-level rectifying column is connected with the discharging opening 22 of adsorption column.
Two-stage rectification tower 4, is connected with the one-level rectifying column 3, and the two-stage rectification tower 4 is used to carry out two-stage rectification removing
Heavy constituent, obtains dichlorosilane.Specifically, the charging aperture 41 of two-stage rectification tower is connected with the tower reactor 33 of one-level rectifying column.
Light component chlorosilane after adsorption-edulcoration is further purified by removal of impurities by one-level rectifying column 3 and two-stage rectification tower 4,
High and low boiling point component therein is separated, while the impurity between dichloro hydrogen silicon and the boiling point of trichlorosilane is entered
Row concentrating and separating.One-level rectifying column 3 is removed in the form of low boiling impurities removal by the tower top 32 of one-level rectifying column and removed by absorption
The light component impurity in light component chlorosilane after miscellaneous, the material produced by the tower reactor 33 of one-level rectifying column enters two grades of essences
Evaporate in tower 4, two-stage rectification tower 4 removes heavy constituent, the restructuring by the tower reactor 43 of two-stage rectification tower in the form of higher boiling impurities removal
Contain substantial amounts of trichlorosilane in point, these trichlorosilanes further purify removal of impurities into downstream purification separator, and two
The tower top 42 of level rectifying column then produces the relatively good high-purity dichlorosilane of quality by way of reflux-withdrawal.
The dichlorosilane that the tower top 42 of two-stage rectification tower is produced can be passed into dirty refining trichlorosilane storage tank 5,
By adjusting the amount into the dichlorosilane of each refining trichlorosilane storage tank 5, to the dichloro in refining trichlorosilane storage tank 5
The accounting of dihydro silicon is adjusted, to carry out also original production polysilicon.Dichlorosilane is in the also reaction of original production polysilicon
Play certain positive facilitation.
Two stage rectification is carried out by the chlorosilane after the absorption of 2 pairs of adsorption column, while improving DCS purity will between DCS with
Impurity between trichlorosilane separate removing；
Preferably, temperature when being parsed in the Analytic Tower 1 is -50~160 DEG C, and pressure is 0.5~1.2MPa.
When being parsed, the mass content accounting of the dichlorosilane in the light component chlorosilane of the enrichment of tower top 11 of Analytic Tower is
20%~50%, produced after the tower top 11 of Analytic Tower is condensed with liquid form；The heavy constituent chlorine being enriched with the tower reactor of Analytic Tower 1
The mass content accounting of dichlorosilane in silane is 0~2%, is discharged downstream purification ＆ isolation device.
Preferably, the temperature of the tower top 11 of the Analytic Tower is -30~-10 DEG C.Specifically, the charging aperture 21 of adsorption column
It is connected with the tower top 11 of Analytic Tower, analytically the low temperature light component chlorosilane for the liquid phase state that the tower top 11 of tower is discharged is entered through
The charging aperture 21 of adsorption column is entered in adsorption column 2, by effectively using Analytic Tower tower top 11 discharge liquid phase state it is light
The cold that component chlorosilane is carried, the impurity for reducing the adsorbent in the running temperature of adsorption column 2, increase adsorption column 2 removes effect
Really.
Preferably, the composition of the adsorbent in the adsorption column 2 includes：The silicon of 20%~60% mass percent
The activated carbon of glue, the aluminum oxide of 10%~30% mass percent and 10%~70% mass percent.Specifically, absorption
The charging aperture 21 of post is connected with the tower top 11 of Analytic Tower.The liquid phase low temperature light component chlorosilane that analytically tower top 11 of tower is produced enters
Enter into adsorption column 2, carrying out absorption by above-mentioned adsorbent removes the impurity containing boron phosphorus.Impurity containing boron phosphorus is mainly three
Boron chloride, the boiling point of boron chloride is 12 DEG C, and the boiling point of dichlorosilane is 8.3 DEG C, and trichlorosilane boiling point is 31.8 DEG C, is contained
The boiling point of the impurity of boron phosphorus is between dichlorosilane and the boiling point of trichlorosilane, in the prior art, generally passes through rectifying
Mode separates dichloro hydrogen silicon and trichlorosilane, can not generally remove boron chloride, and the present embodiment is then given birth to by polycrystalline reduction
The retracting device of the dichlorosilane in tail gas in production removes boron chloride.
Preferably, the pressure when one-level rectifying column 3 carries out rectifying is 0.4~0.5MPa.Pass through one-level rectifying column 3
Rectifying be dissolved in hydrogen chloride in the chlorosilane after adsorption-edulcoration and remove, the fixed gas of the tower top 32 of one-level rectifying column
Discharges material includes：The hydrogen chloride of 80%~90% mass percent, the dichlorosilane of 1%~2% mass percent；One-level
The liquid phase extraction material of the tower top 32 of rectifying column includes：The hydrogen chloride of 10%~15% mass percent, 5%~10% matter
Measure the dichlorosilane of percentage；The extraction material of tower reactor 33 of one-level rectifying column includes：90%~95% mass percent
Dichlorosilane, continues to purify removal of impurities into two-stage rectification tower 4.
Preferably, the pressure when two-stage rectification tower 4 carries out rectifying is 0.4~0.5MPa.Pass through two-stage rectification tower 4
Rectifying, two-stage rectification tower tower reactor 43 extraction material include：The dichlorosilane of 10%~15% mass percent, 90%
The trichlorosilane of~95% mass percent, into the further separating-purifying of downstream purification separator；Two-stage rectification tower
The fixed gas discharges material of tower top 42 includes：The dichlorosilane and a small amount of trichlorosilane of 2%~6% quality percentage, two grades
The liquid phase of the tower top 42 extraction material of rectifying column includes：The trichlorosilane of 1%~2% mass percent, 60%~80%%
The dichlorosilane of mass percent.
Preferably, the one-level rectifying column 3, two-stage rectification tower 4 are non-metallic fillers tower, and the non-metallic fillers tower is
Inner liner polytetrafluoroethylene packed tower, so as to avoid the dichloro two that metal impurities are brought into the tail gas in polycrystalline reduction production
In the retracting device of hydrogen silicon.
By the temperature and pressure for controlling to be parsed in Analytic Tower 1, the tail gas parsing point during polycrystalline reduction is produced
From in the isolated low temperature chlorosilane for occupying larger proportion of the tower top 11 of Analytic Tower, and the chlorosilane is the low temperature shape of liquid phase
The chlorosilane of state, hydrogen chloride is obtained in the tower reactor 12 of Analytic Tower.The chlorosilane of the low-temperature condition of liquid phase is passed through and is filled with absorption
In the adsorption column 2 of agent, absorption is carried out to the impurity containing boron phosphorus in the chlorosilane of the low-temperature condition of liquid phase under cryogenic de-
Remove, the chlorosilane after adsorption-edulcoration enters further impurity removal in the one-level rectifying column 3 and two-stage rectification tower 4 in downstream.
By control polycrystalline reduction produce in tail gas in dichlorosilane retracting device the pressure of Analytic Tower 1 and
Temperature, the tail gas parsing separation during polycrystalline reduction is produced, in the isolated larger proportion that occupies of the tower top 11 of Analytic Tower
Low temperature chlorosilane, and the chlorosilane is the chlorosilane of the low-temperature condition of liquid phase, and high temperature heavy constituent is obtained in the tower reactor 12 of Analytic Tower
Chlorosilane.The chlorosilane of the low-temperature condition of liquid phase is passed through in the adsorption column 2 for being filled with adsorbent, under cryogenic to liquid phase
Low-temperature condition chlorosilane in impurity containing boron phosphorus carry out adsorbing and removing, the chlorosilane after adsorption-edulcoration is entered down
Further removal of impurities in the one-level rectifying column 3 and two-stage rectification tower 4 of trip.Preferably, the polycrystalline reduction life in the present embodiment
The retracting device of the dichlorosilane in tail gas in production also includes heat integration heat exchanger, is entering one-level rectifying column 3
Before first pass through heat integration heat exchanger and enter the pre-heat treatment, be close to bubble point feed state, reach energy-saving effect
Really.
The transmission of corresponding heat and quality is carried out into each component that the boiling point of one-level rectifying column 3 has differences, simultaneously
The high low boiling impurity of trace level is effectively carried to the tower reactor 33 of the tower top 32 and one-level rectifying column to one-level rectifying column.One
The tower top 32 of level rectifying column is discharged into downstream purification separator, the tower reactor 33 of one-level rectifying column in the form of low boiling impurities removal
The high boiling material that contains of discharge enters two-stage rectification tower 4, and the tower reactor 43 by two-stage rectification tower of two-stage rectification tower 4 is with height
Enter downstream process after the form removing heavy constituent of boiling point impurities removal and carry out batch operation.
Specifically, by high-purity dichlorosilane and refining trichlorosilane dispensing, dichloro-dihydro silicone content is allocated in quality
Between percentage 1%~10%, reach after the required uniform batch mixing purpose of reduction production, stability contorting ratio for reduction
Reaction produces polysilicon.In reduction furnace, polysilicon growth process：Trichlorosilane participates in the reaction equation of reduction reaction：
SiHCl3(g)+H2=Si+3HCl (g)；Dichlorosilane participates in the chemical equation of reaction：SiH2Cl2(g)=Si (s)+
2HCl (g), dichlorosilane participates in the Gibbs free energy of reaction closer to negative value, and the anti-of reduction reaction is participated in than trichlorosilane
Answer equation：SiHCl3(g)+H2=Si+3HCl (g) is easier to occur.Mean that dichlorosilane is easier the conversion that reacts
For polysilicon.Therefore, mixed with a certain proportion of dichlorosilane in refining trichlorosilane, effective recycling two is not only acted as
The effect of chlorine dihydro silicon, while conversion ratio of reduction can be lifted significantly.
Pass through the retracting device of the dichlorosilane in the tail gas in the polycrystalline reduction production in the present embodiment, it is not necessary to
Substantial amounts of alkali lye and water are consumed, dichloro can just be obtained by Analytic Tower 1, adsorption column 2, one-level rectifying column 3, two-stage rectification tower 4
Dihydro silicon, vent gas treatment cost is low, and pollution is few.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, but the invention is not limited in this.For those skilled in the art, the essence of the present invention is not being departed from
In the case of refreshing and essence, various changes and modifications can be made therein, and these variations and modifications are also considered as protection scope of the present invention.
Claims (12)
1. the recovery method of the dichlorosilane in tail gas in a kind of polycrystalline reduction production, it is characterised in that including following
Step：
(1) tail gas during polycrystalline reduction is produced carries out parsing separation, the hydrogen chloride and chlorine separated by Analytic Tower
Silane, the light component chlorosilane of the tower top of Analytic Tower is condensed into liquid phase state；
(2) impurity containing boron phosphorus is removed in the light component chlorosilane progress absorption to liquid phase state；
(3) one-level rectifying removing light component is carried out；
(4) two-stage rectification removing heavy constituent is carried out, dichlorosilane is obtained.
2. the recovery method of the dichlorosilane in tail gas in polycrystalline reduction production according to claim 1, it is special
Levy and be, in the step (1), the temperature of the parsing is -50~160 DEG C, and the pressure of the parsing is 0.5~1.2MPa.
3. the recovery method of the dichlorosilane in tail gas in polycrystalline reduction production according to claim 1, it is special
Levy and be, in the step (1), the temperature for parsing the chlorosilane separated is -30~-10 DEG C.
4. the recovery method of the dichlorosilane in tail gas in polycrystalline reduction production according to claim 1, it is special
Levy and be, in the step (2), the composition of the adsorbent used when being adsorbed includes：20%~60% quality hundred
Divide the activated carbon of the silica gel, the aluminum oxide of 10%~30% mass percent and 10%~70% mass percent of ratio.
5. the recovery method of the dichlorosilane in tail gas in polycrystalline reduction production according to claim 1, it is special
Levy and be, in the step (3), the pressure for carrying out one-level rectifying is 0.4~0.5MPa.
6. the recovery method of the dichlorosilane in tail gas in polycrystalline reduction production according to claim 1, it is special
Levy and be, in the step (4), the pressure for carrying out two-stage rectification is 0.4~0.5MPa.
7. a kind of retracting device of the dichlorosilane in tail gas in polycrystalline reduction production, it is characterised in that including：
Analytic Tower, for polycrystalline reduction to be produced in tail gas carry out parsing separation, the hydrogen chloride separated and chlorine silicon
Alkane, the light component chlorosilane of the tower top of Analytic Tower is condensed into liquid phase state；
Adsorption column, is connected with the Analytic Tower, and the light component chlorosilane progress absorption that the adsorption column is used for liquid phase state is removed
Fall the impurity containing boron phosphorus；
One-level rectifying column, is connected with the adsorption column, and the one-level rectifying column is used to carry out one-level rectifying removing light component；
Two-stage rectification tower, is connected with the one-level rectifying column, and the two-stage rectification tower is used to carry out two-stage rectification removing heavy constituent,
Obtain dichlorosilane.
8. the retracting device of the dichlorosilane in tail gas in polycrystalline reduction production according to claim 7, it is special
Levy and be, temperature when being parsed in the Analytic Tower is -50~160 DEG C, pressure is 0.5~1.2MPa
9. the retracting device of the dichlorosilane in tail gas in polycrystalline reduction production according to claim 7, it is special
Levy and be, the temperature of the tower top of the Analytic Tower is -30~-10 DEG C.
10. the retracting device of the dichlorosilane in tail gas in polycrystalline reduction production according to claim 7, it is special
Levy and be, the composition of the adsorbent in the adsorption column includes：The silica gel of 20%~60% mass percent, 10%~30%
Mass percent aluminum oxide and the activated carbon of 10%~70% mass percent.
11. the retracting device of the dichlorosilane in tail gas in polycrystalline reduction production according to claim 7, it is special
Levy and be, the pressure when one-level rectifying column carries out rectifying is 0.4~0.5MPa.
12. the retracting device of the dichlorosilane in tail gas in polycrystalline reduction production according to claim 7, it is special
Levy and be, the pressure when two-stage rectification tower carries out rectifying is 0.4~0.5MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410484800.5A CN105480981B (en) | 2014-09-19 | 2014-09-19 | The recovery method and device of a kind of dichlorosilane in tail gas in polycrystalline reduction production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410484800.5A CN105480981B (en) | 2014-09-19 | 2014-09-19 | The recovery method and device of a kind of dichlorosilane in tail gas in polycrystalline reduction production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105480981A CN105480981A (en) | 2016-04-13 |
| CN105480981B true CN105480981B (en) | 2017-09-26 |
Family
ID=55668316
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410484800.5A Active CN105480981B (en) | 2014-09-19 | 2014-09-19 | The recovery method and device of a kind of dichlorosilane in tail gas in polycrystalline reduction production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105480981B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107720759A (en) * | 2017-11-13 | 2018-02-23 | 亚洲硅业（青海）有限公司 | The processing method of tail gas is reduced in a kind of preparation method and production of polysilicon of optical fiber level silicon tetrachloride |
| CN111036029B (en) * | 2018-10-15 | 2022-03-04 | 新特能源股份有限公司 | Method for recovering waste gas in polycrystalline silicon production process |
| CN109573950A (en) * | 2019-01-31 | 2019-04-05 | 内蒙古通威高纯晶硅有限公司 | A kind of Analytic Tower hydrogen chloride recovery system and technique |
| CN113024593A (en) * | 2019-12-24 | 2021-06-25 | 新特能源股份有限公司 | Dimethyl dichlorosilane, preparation method and preparation device thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102389687A (en) * | 2011-09-28 | 2012-03-28 | 四川瑞能硅材料有限公司 | Method for promoting purity of chlorine hydride recycled by reduction unit of polysilicon tail gas separating system |
| EP2481708A1 (en) * | 2011-02-01 | 2012-08-01 | Wacker Chemie AG | Process for purifying chlorosilanes by distillation |
| CN102614741A (en) * | 2012-03-31 | 2012-08-01 | 四川新光硅业科技有限责任公司 | Tail gas recovery processing method for polycrystalline silicon production |
| CN103342341A (en) * | 2013-07-19 | 2013-10-09 | 新特能源股份有限公司 | Tail gas separation process in polycrystalline silicon production |
| CN103466634A (en) * | 2013-09-03 | 2013-12-25 | 新特能源股份有限公司 | Energy-saving process for recycling mixed chlorosilane raw material in production of polycrystalline silicon |
| CN103896278A (en) * | 2012-12-31 | 2014-07-02 | 天津市泰亨气体有限公司 | Preparation method for preparing dichlorosilane by adopting recovery method |
-
2014
- 2014-09-19 CN CN201410484800.5A patent/CN105480981B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2481708A1 (en) * | 2011-02-01 | 2012-08-01 | Wacker Chemie AG | Process for purifying chlorosilanes by distillation |
| CN102389687A (en) * | 2011-09-28 | 2012-03-28 | 四川瑞能硅材料有限公司 | Method for promoting purity of chlorine hydride recycled by reduction unit of polysilicon tail gas separating system |
| CN102614741A (en) * | 2012-03-31 | 2012-08-01 | 四川新光硅业科技有限责任公司 | Tail gas recovery processing method for polycrystalline silicon production |
| CN103896278A (en) * | 2012-12-31 | 2014-07-02 | 天津市泰亨气体有限公司 | Preparation method for preparing dichlorosilane by adopting recovery method |
| CN103342341A (en) * | 2013-07-19 | 2013-10-09 | 新特能源股份有限公司 | Tail gas separation process in polycrystalline silicon production |
| CN103466634A (en) * | 2013-09-03 | 2013-12-25 | 新特能源股份有限公司 | Energy-saving process for recycling mixed chlorosilane raw material in production of polycrystalline silicon |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105480981A (en) | 2016-04-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105480981B (en) | The recovery method and device of a kind of dichlorosilane in tail gas in polycrystalline reduction production | |
| CN102249187B (en) | System and process for recovering pure hydrogen and liquid HCl through polysilicon tail gas treatment | |
| WO2020103799A1 (en) | Device and method for removing methyldichlorosilane from trichlorosilane by means of reactive distillation | |
| CN112340703B (en) | Method for preparing anhydrous hydrogen fluoride and nano silicon dioxide by using fluosilicic acid | |
| CN113247908B (en) | Separation method and separation device for chlorosilane in polysilicon production | |
| CN101538044A (en) | System for separating and purifying trichlorosilane in production process of polysilicon and operation method thereof | |
| CN105036081A (en) | Method for producing HCl gas through chlorosilane residual liquor | |
| CN102701216B (en) | Impurity removing method for dichlorosilane | |
| CN115838175A (en) | Method and system for removing carbon impurities in chlorosilane | |
| CN101376499B (en) | Method for preparing polysilicon | |
| CN110963494A (en) | System and method for preparing silane | |
| CN106698438B (en) | Coupled polycrystalline silicon production system | |
| CN219730550U (en) | Chlorosilane rectifying and impurity removing system in polysilicon production | |
| CN101372336B (en) | Method for preparing polysilicon | |
| CN104262376A (en) | TMSOTf (trimethylsilyl trifluoromethanesulfonate) purifying method | |
| CN101913609A (en) | Method and device for removing impurities from trichlorosilane mixed gas | |
| CN115006861B (en) | System and process for separating polycrystalline silicon reduction tail gas absorption rich liquid and condensate | |
| CN108502889A (en) | The separation of polysilicon cold hydrogenation product and purifying plant and method | |
| CN102795629B (en) | Method for purification of dichlorosilane from dry method recovered material | |
| CN217458845U (en) | System for increasing reaction efficiency of polycrystalline silicon reduction furnace | |
| CN114956092A (en) | Method for separating monomethyldichlorosilane impurities from trichlorosilane | |
| CN105366681B (en) | The also treating method and apparatus of the chlorosilane of original production polysilicon recovery, the processing method and system of chlorosilane in production of polysilicon | |
| CN108946742A (en) | Purify the device of trichlorosilane | |
| CN111268682B (en) | Composition for preparing polycrystalline silicon, preparation method and preparation system | |
| CN212864156U (en) | Impurity removing device for polycrystalline silicon reduction tail gas |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20160413 Assignee: Xinte silicon based new materials Co.,Ltd. Assignor: XINTE ENERGY Co.,Ltd. Contract record no.: X2023990000586 Denomination of invention: A method and device for recovering dichlorosilane from tail gas in polycrystalline silicon reduction production Granted publication date: 20170926 License type: Common License Record date: 20230605 |