CN105480981A - Method and device for recovering dichlorosilane from tail gas in reduction production of polysilicon - Google Patents
Method and device for recovering dichlorosilane from tail gas in reduction production of polysilicon Download PDFInfo
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- CN105480981A CN105480981A CN201410484800.5A CN201410484800A CN105480981A CN 105480981 A CN105480981 A CN 105480981A CN 201410484800 A CN201410484800 A CN 201410484800A CN 105480981 A CN105480981 A CN 105480981A
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Abstract
The invention discloses a method and a device for recovering dichlorosilane from tail gas in reduction production of polysilicon. The method comprises the following steps: (1) subjecting the tail gas in reduction production of polysilicon to resolution and separation so as to obtain separated hydrogen chloride and chlorosilane; (2) subjecting obtained chlorosilane to adsorption so as to remove impurities containing boron and phosphorus; (3) carrying out first-grade rectification so as to remove light fractions; and (4) carrying out second-grade rectification so as to remove heavy fractions and obtain dichlorosilane. The method provided by the invention does not need to consume a great amount of alkali liquor and water, can obtain dichlorosilane through the processes of resolution, adsorption, first-grade rectification and second-grade rectification, and has low cost and little pollution in treatment of the tail gas.
Description
Technical field
The invention belongs to technical field of polysilicon production, be specifically related to recovery method and the device of the dichlorosilane in the tail gas in the production of a kind of polycrystalline reduction.
Background technology
Polysilicon enterprise can produce a large amount of tail gas, the discharge rate average out to 5000 ~ 10000NM of tail gas in polycrystalline reduction is produced
3/ h.The main component of above-mentioned tail gas comprises: the phosphorus trichloride of silicon tetrachloride, trichlorosilane, dichlorosilane, hydrogenchloride, hydrogen and trace, phosphorus pentachloride, boron trichloride, borine, phosphine and metal chloride (wherein, phosphorus trichloride, phosphorus pentachloride, boron trichloride, borine, phosphine and metal chloride are trace) etc.Under normal circumstances, these tail gas all can be sent to raffinate device, adopt alkali lye to carry out drip washing to tail gas, then by entering air after washing.Chlorosilane gas major part in tail gas is neutralized under alkali lye drip washing state, and the material after neutralization is fed to pressure filter press filtration and obtains waste residue, and waste residue is delivered to the external world and processed.And consuming a large amount of alkali lye and water in above-mentioned vent gas treatment process, vent gas treatment cost is higher.
Summary of the invention
Technical problem to be solved by this invention is for above shortcomings in prior art, the recovery method of the dichlorosilane in the tail gas in providing a kind of polycrystalline reduction to produce and device, the method treating processes is simple, does not use alkali lye and water, effectively can obtain dichlorosilane.
The technical scheme that solution the technology of the present invention problem adopts is to provide the recovery method of the dichlorosilane in the tail gas in the production of a kind of polycrystalline reduction, comprises the following steps:
(1) tail gas in polycrystalline reduction being produced carries out parsings separation, obtains the hydrogenchloride separated and chlorosilane;
(2) described chlorosilane is adsorbed to the impurity removed containing boron phosphorus;
(3) carry out one-level rectifying and remove light constituent;
(4) carry out two-stage rectification and remove heavy constituent, obtain dichlorosilane.
Preferably, in described step (1), the temperature of described parsing is-50 ~ 160 DEG C, and the pressure of described parsing is 0.5 ~ 1.2MPa.
Preferably, in described step (1), the temperature of the chlorosilane that described parsing is separated is-30 ~-10 DEG C.
Preferably, in described step (2), described in the composition of sorbent material used when adsorbing comprise: the gac of the silica gel of mass percent of 20% ~ 60%, the aluminum oxide of the mass percent of 10% ~ 30% and the mass percent of 10% ~ 70%.
Preferably, in described step (3), described in carry out one-level rectifying pressure be 0.4 ~ 0.5MPa.
Preferably, in described step (4), described in carry out two-stage rectification pressure be 0.4 ~ 0.5MPa.
The invention provides the retrieving arrangement of the dichlorosilane in the tail gas in the production of a kind of polycrystalline reduction, comprising:
Analytic Tower, carries out parsings separation for the tail gas in polycrystalline reduction being produced, obtains the hydrogenchloride separated and chlorosilane;
Adsorption column, is connected with described Analytic Tower, and described adsorption column is used for adsorbing to described chlorosilane the impurity removed containing boron phosphorus;
One-level rectifying tower, is connected with described adsorption column, and described one-level rectifying tower is used for carrying out one-level rectifying and removes light constituent;
Two-stage rectification tower, is connected with described one-level rectifying tower, and described two-stage rectification tower is used for carrying out two-stage rectification and removes heavy constituent, obtains dichlorosilane.
Preferably, temperature when resolving in described Analytic Tower is-50 ~ 160 DEG C, and pressure is 0.5 ~ 1.2MPa
Preferably, the temperature of the tower top of described Analytic Tower is-30 ~-10 DEG C.
Preferably, the composition of the sorbent material in described adsorption column comprises: the gac of the silica gel of mass percent of 20% ~ 60%, the aluminum oxide of the mass percent of 10% ~ 30% and the mass percent of 10% ~ 70%.
Preferably, pressure when described one-level rectifying tower carries out rectifying is 0.4 ~ 0.5MPa.
Preferably, pressure when described two-stage rectification tower carries out rectifying is 0.4 ~ 0.5MPa.
Preferably, described one-level rectifying tower, described two-stage rectification tower are non-metallic fillers tower, and are inner liner polytetrafluoroethylene packing tower.
The recovery method of the dichlorosilane in the tail gas in being produced by the polycrystalline reduction in the present invention and device, do not need to consume a large amount of alkali lye and water, can pass through parsing, absorption, one-level rectifying, two-stage rectification process just obtain dichlorosilane, vent gas treatment cost is low, pollutes few.
Accompanying drawing explanation
Fig. 1 is the structural representation of retrieving arrangement of the dichlorosilane in the crystal silicon reduction tail gas in the embodiment of the present invention 2.
In figure: 1-Analytic Tower; The tower top of 11-Analytic Tower; The tower reactor of 12-Analytic Tower; 2-adsorption column; The opening for feed of 21-adsorption column; The discharge port of 22-adsorption column; 3-one-level rectifying tower; The opening for feed of 31-one-level rectifying tower; The tower top of 32-one-level rectifying tower; The tower reactor of 33-one-level rectifying tower; 4-two-stage rectification tower; The opening for feed of 41-two-stage rectification tower; The tower top of 42-two-stage rectification tower; The tower reactor of 43-two-stage rectification tower; 5-refining trichlorosilane storage tank.
Embodiment
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Embodiment 1
The recovery method of the dichlorosilane in the tail gas during the present embodiment provides a kind of polycrystalline reduction to produce, comprises the following steps:
(1) tail gas in polycrystalline reduction being produced carries out parsings separation, obtains the hydrogenchloride separated and chlorosilane;
(2) described chlorosilane is adsorbed to the impurity removed containing boron phosphorus;
(3) carry out one-level rectifying and remove light constituent;
(4) carry out two-stage rectification and remove heavy constituent, obtain dichlorosilane.
Preferably, in described step (1), the temperature of described parsing is-50 ~ 160 DEG C, and the pressure of described parsing is 0.5 ~ 1.2MPa.
Preferably, in described step (1), the temperature of the chlorosilane that described parsing is separated is-30 ~-10 DEG C.
Preferably, in described step (2), described in the composition of sorbent material used when adsorbing comprise: the gac of the silica gel of mass percent of 20% ~ 60%, the aluminum oxide of the mass percent of 10% ~ 30% and the mass percent of 10% ~ 70%.
Preferably, in described step (3), described in carry out one-level rectifying pressure be 0.4 ~ 0.5MPa.
Preferably, in described step (4), described in carry out two-stage rectification pressure be 0.4 ~ 0.5MPa.
The recovery method of the dichlorosilane in the tail gas in being produced by the polycrystalline reduction in the present embodiment, do not need to consume a large amount of alkali lye and water, can pass through parsing, absorption, one-level rectifying, two-stage rectification process just obtain dichlorosilane, vent gas treatment cost is low, pollutes few.
Embodiment 2
As shown in Figure 1, the retrieving arrangement of the dichlorosilane in the tail gas during the present embodiment provides a kind of polycrystalline reduction to produce, comprising:
Analytic Tower 1, carries out parsings separation for the tail gas in polycrystalline reduction being produced, obtains the hydrogenchloride separated and chlorosilane.Described Analytic Tower 1 is specially hydrogenchloride rich solution knockout tower, is separated by the hydrogenchloride be dissolved in chlorosilane.Pre-separation can be carried out by Analytic Tower 1 pair of chlorosilane, reduce the production load of downstream purification tripping device.
Polycrystalline reduction produce in tail gas mainly comprise the phosphorus trichloride of silicon tetrachloride, trichlorosilane, dichlorosilane, hydrogenchloride, hydrogen and trace, phosphorus pentachloride, boron trichloride, borine, phosphine and metal chloride (wherein, phosphorus trichloride, phosphorus pentachloride, boron trichloride, borine, phosphine and metal chloride are trace).The boiling point of hydrogenchloride is lower (under atmospheric pressure state, boiling point is-85 DEG C), the boiling-point difference of it and chlorosilane apart from large, so parsings separation can be carried out by Analytic Tower 1.After tail gas in polycrystalline reduction being produced carries out parsings separation by Analytic Tower 1, usual hydrogenchloride arranges separation outward with the interchanger of the form of the non-condensable gas analytically tower top 11 of tower; Simultaneously, the light constituent chlorosilane (being mainly dichlorosilane and trichlorosilane) that tower top 11 enrichment of Analytic Tower is more, the light constituent chlorosilane of the tower top 11 of Analytic Tower is condensed into liquid phase state, and light constituent chlorosilane is got back in Analytic Tower 1 by the liquid-phase reflux pipeline of the tower top 11 of Analytic Tower and set up circulation; Analytically the light constituent chlorosilane of a tributary stock extraction liquid phase state drawn by the liquid-phase reflux pipeline of the tower top 11 of tower, the tower reactor 12 of Analytic Tower is heavy constituent chlorosilane rich region, enters downstream purification tripping device after tower reactor 12 extraction of heavy constituent chlorosilane analytically tower.The mixture of trichlorosilane, dichlorosilane and a small amount of hydrogenchloride is mainly comprised in the light constituent chlorosilane of liquid phase state.
The pre-separation of the tail gas in polycrystalline reduction production is tentatively completed in Analytic Tower 1, when chlorosilane total amount is constant, by the tower top 11 extraction liquid phase low temperature light constituent chlorosilane of Analytic Tower, the heavy constituent chlorosilane reducing tower reactor 12 extraction of Analytic Tower enters the chlorosilane amount of downstream purification tripping device, alleviate the removal of impurities segregational load of downstream purification device, especially, under production oepration at full load state, this step seems particularly important.
Adsorption column 2, is connected with described Analytic Tower 1, and described adsorption column 2 is for adsorbing the impurity removed containing boron phosphorus to described chlorosilane.Concrete, the opening for feed 21 of adsorption column is connected with the tower top 11 of Analytic Tower.After adsorption column 2, obtain the light constituent chlorosilane after adsorption-edulcoration.Concrete, the adsorption column 2 in the present embodiment is for being filled with the chlorosilane treating plant of sorbent material, and this equipment can by the trace B phosphorus impurities adsorbing and removing in liquid-phase chlorosilane.
One-level rectifying tower 3, is connected with described adsorption column 2, and described one-level rectifying tower 3 removes light constituent for carrying out one-level rectifying.Concrete, the opening for feed 31 of one-level rectifying tower is connected with the discharge port 22 of adsorption column.
Two-stage rectification tower 4, is connected with described one-level rectifying tower 3, and described two-stage rectification tower 4 removes heavy constituent for carrying out two-stage rectification, obtains dichlorosilane.Concrete, the opening for feed 41 of two-stage rectification tower is connected with the tower reactor 33 of one-level rectifying tower.
Light constituent chlorosilane after adsorption-edulcoration to be purified further removal of impurities by one-level rectifying tower 3 and two-stage rectification tower 4, high and low boiling point component is wherein separated, the impurity between dichloro hydrogen silicon and the boiling point of trichlorosilane is carried out concentrating and separating simultaneously.One-level rectifying tower 3 to remove the light constituent impurity in the light constituent chlorosilane after adsorption-edulcoration with the form of lower boiling impurities removal by the tower top 32 of one-level rectifying tower, enter in two-stage rectification tower 4 by the material of tower reactor 33 extraction of one-level rectifying tower, two-stage rectification tower 4 removes heavy constituent by the tower reactor 43 of two-stage rectification tower with the form of high boiling point impurities removal, containing a large amount of trichlorosilanes in this heavy constituent, these trichlorosilanes enter downstream purification tripping device and to purify further removal of impurities, at the tower top 42 of two-stage rectification tower then by dichlorosilane that the mode extraction quality of reflux-withdrawal is high-purity relatively preferably.
The dichlorosilane of tower top 42 extraction of two-stage rectification tower can be passed into dirty refining trichlorosilane storage tank 5, by regulating the amount entering the dichlorosilane of each refining trichlorosilane storage tank 5, the accounting of the dichlorosilane in refining trichlorosilane storage tank 5 is adjusted, carries out also original production polysilicon.Dichlorosilane plays certain forward promoter action in the reaction of going back original production polysilicon.
By adsorption column 2, two stage rectification is carried out to the chlorosilane after absorption, while improving DCS purity, the impurity between DCS with trichlorosilane is carried out being separated removal;
Preferably, temperature when resolving in described Analytic Tower 1 is-50 ~ 160 DEG C, and pressure is 0.5 ~ 1.2MPa.When resolving, the mass content accounting of the dichlorosilane in the light constituent chlorosilane of tower top 11 enrichment of Analytic Tower is 20% ~ 50%, with liquid form extraction after tower top 11 condensation of Analytic Tower; The mass content accounting of the dichlorosilane in the heavy constituent chlorosilane of the tower reactor enrichment of Analytic Tower 1 is 0 ~ 2%, enters downstream purification tripping device.
Preferably, the temperature of the tower top 11 of described Analytic Tower is-30 ~-10 DEG C.Concrete, the opening for feed 21 of adsorption column is connected with the tower top 11 of Analytic Tower, the opening for feed 21 that the low temperature light constituent chlorosilane of liquid phase state that analytically tower top 11 of tower is discharged enters through adsorption column enters into adsorption column 2, the cold that the light constituent chlorosilane of the liquid phase state of discharging by effectively utilizing the tower top 11 of Analytic Tower carries, reduce the operating temperature of adsorption column 2, increase the Impurity removal effect of the sorbent material in adsorption column 2.
Preferably, the composition of the sorbent material in described adsorption column 2 comprises: the gac of the silica gel of mass percent of 20% ~ 60%, the aluminum oxide of the mass percent of 10% ~ 30% and the mass percent of 10% ~ 70%.Concrete, the opening for feed 21 of adsorption column is connected with the tower top 11 of Analytic Tower.Analytically the liquid phase low temperature light constituent chlorosilane of tower top 11 extraction of tower enters into adsorption column 2, is undertaken adsorbing the impurity removed containing boron phosphorus by above-mentioned sorbent material.Impurity containing boron phosphorus is mainly boron trichloride, the boiling point of boron trichloride is 12 DEG C, the boiling point of dichlorosilane is 8.3 DEG C, trichlorosilane boiling point is 31.8 DEG C, the boiling point of the impurity containing boron phosphorus is between dichlorosilane and the boiling point of trichlorosilane, in prior art, usually dichloro hydrogen silicon and trichlorosilane is separated by the mode of rectifying, usually cannot remove boron trichloride, the present embodiment then produced by polycrystalline reduction in tail gas in the retrieving arrangement of dichlorosilane boron trichloride is removed.
Preferably, pressure when described one-level rectifying tower 3 carries out rectifying is 0.4 ~ 0.5MPa.By the hydrogenchloride removing that the rectifying of one-level rectifying tower 3 will be dissolved in the chlorosilane after adsorption-edulcoration, the non-condensable gas discharges material of the tower top 32 of one-level rectifying tower comprises: the hydrogenchloride of 80% ~ 90% mass percent, the dichlorosilane of 1% ~ 2% mass percent; The liquid phase extraction material of the tower top 32 of one-level rectifying tower comprises: the hydrogenchloride of the mass percent of 10% ~ 15%, the dichlorosilane of the mass percent of 5% ~ 10%; The tower reactor 33 extraction material of one-level rectifying tower comprises: the dichlorosilane of the mass percent of 90% ~ 95%, enters two-stage rectification tower 4 and continue purification removal of impurities.
Preferably, pressure when described two-stage rectification tower 4 carries out rectifying is 0.4 ~ 0.5MPa.By the rectifying of two-stage rectification tower 4, the tower reactor 43 extraction material of two-stage rectification tower comprises: the dichlorosilane of the mass percent of 10% ~ 15%, and the trichlorosilane of the mass percent of 90% ~ 95%, enters the further separating-purifying of downstream purification tripping device; The tower top 42 non-condensable gas discharges material of two-stage rectification tower comprises: the dichlorosilane of the percent mass of 2% ~ 6% and a small amount of trichlorosilane, the tower top 42 liquid phase extraction material of two-stage rectification tower comprises: the trichlorosilane of the mass percent of 1% ~ 2%, the dichlorosilane of the mass percent of 60% ~ 80%%.
Preferably, described one-level rectifying tower 3, two-stage rectification tower 4 are non-metallic fillers tower, this non-metallic fillers tower is inner liner polytetrafluoroethylene packing tower, thus can avoid metallic impurity bring into polycrystalline reduction produce in tail gas in dichlorosilane retrieving arrangement in.
By controlling the temperature and pressure carrying out in Analytic Tower 1 resolving, tail gas in polycrystalline reduction being produced is resolved and is separated, be separated at the tower top 11 of Analytic Tower and obtain the low temperature chlorosilane occupying larger proportion, and this chlorosilane is the chlorosilane of the low-temperature condition of liquid phase, obtain hydrogenchloride in the tower reactor 12 of Analytic Tower.Being passed into by the chlorosilane of the low-temperature condition of liquid phase is filled with in the adsorption column 2 of sorbent material, carry out adsorbing and removing to the impurity containing boron phosphorus in the chlorosilane of the low-temperature condition of liquid phase under cryogenic, the chlorosilane after adsorption-edulcoration enters into one-level rectifying tower 3 and the two-stage rectification tower 4 further impurity removal in downstream.
By controlling Analytic Tower 1 pressure and the temperature of the retrieving arrangement of the dichlorosilane in the tail gas in polycrystalline reduction production, tail gas in polycrystalline reduction being produced is resolved and is separated, be separated at the tower top 11 of Analytic Tower and obtain the low temperature chlorosilane occupying larger proportion, and this chlorosilane is the chlorosilane of the low-temperature condition of liquid phase, obtain high temperature heavy constituent chlorosilane in the tower reactor 12 of Analytic Tower.Being passed into by the chlorosilane of the low-temperature condition of liquid phase is filled with in the adsorption column 2 of sorbent material, carry out adsorbing and removing to the impurity containing boron phosphorus in the chlorosilane of the low-temperature condition of liquid phase under cryogenic, the chlorosilane after adsorption-edulcoration enters into one-level rectifying tower 3 and the two-stage rectification tower 4 further removal of impurities in downstream.Preferably, the retrieving arrangement of the dichlorosilane in the tail gas in the polycrystalline reduction production in the present embodiment also comprises heat integration interchanger, first thermal pretreatment is entered through heat integration interchanger before entering one-level rectifying tower 3, make it close to bubble point feed state, reach energy-saving and cost-reducing effect.
Each component that the boiling point entering one-level rectifying tower 3 there are differences carries out the transmission of corresponding heat and quality, and the impurity that simultaneously boiled by the height of trace level is carried into the tower top 32 of one-level rectifying tower and the tower reactor 33 of one-level rectifying tower effectively.The tower top 32 of one-level rectifying tower is discharged with the form of lower boiling impurities removal and is entered downstream purification tripping device, what the tower reactor 33 of one-level rectifying tower was discharged enters two-stage rectification tower 4 containing high boiling material, two-stage rectification tower 4 remove heavy constituent by the tower reactor 43 of two-stage rectification tower with the form of high boiling point impurities removal after enter downstream process and carry out batch operation.
Concrete, high-purity dichlorosilane and refining trichlorosilane are prepared burden, the allotment of dichloro-dihydro silicone content, between mass percent 1% ~ 10%, reaches the required even batch mixing object of reduction production, produces polysilicon after stability contorting ratio for reduction reaction.In reduction furnace, polysilicon growth process: trichlorosilane participates in the reaction equation of reduction reaction: SiHCl
3(g)+H
2=Si+3HCl (g); Dichlorosilane participates in the chemical equation of reaction: SiH
2cl
2g ()=Si (s)+2HCl (g), dichlorosilane participates in the Gibbs free energy of reaction closer to negative value, participates in the reaction equation of reduction reaction: SiHCl than trichlorosilane
3(g)+H
2=Si+3HCl (g) more easily occurs.Mean that dichlorosilane more easily reacts and be converted into polysilicon.Therefore, in refining trichlorosilane, be mixed with a certain proportion of dichlorosilane, not only play the effect of effective recycling dichlorosilane, reduction transformation efficiency can be promoted significantly simultaneously.
The retrieving arrangement of the dichlorosilane in the tail gas in being produced by the polycrystalline reduction in the present embodiment, do not need to consume a large amount of alkali lye and water, just can obtain dichlorosilane by Analytic Tower 1, adsorption column 2, one-level rectifying tower 3, two-stage rectification tower 4, vent gas treatment cost is low, pollutes few.
Be understandable that, the illustrative embodiments that above embodiment is only used to principle of the present invention is described and adopts, but the present invention is not limited thereto.For those skilled in the art, without departing from the spirit and substance in the present invention, can make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.
Claims (12)
1. a recovery method for the dichlorosilane in the tail gas in polycrystalline reduction production, is characterized in that, comprise the following steps:
(1) tail gas in polycrystalline reduction being produced carries out parsings separation, obtains the hydrogenchloride separated and chlorosilane;
(2) described chlorosilane is adsorbed to the impurity removed containing boron phosphorus;
(3) carry out one-level rectifying and remove light constituent;
(4) carry out two-stage rectification and remove heavy constituent, obtain dichlorosilane.
2. the recovery method of the dichlorosilane in the tail gas in polycrystalline reduction production according to claim 1, it is characterized in that, in described step (1), the temperature of described parsing is-50 ~ 160 DEG C, and the pressure of described parsing is 0.5 ~ 1.2MPa.
3. the recovery method of the dichlorosilane in the tail gas in polycrystalline reduction production according to claim 1, it is characterized in that, in described step (1), the temperature of the chlorosilane that described parsing is separated is-30 ~-10 DEG C.
4. the recovery method of the dichlorosilane in the tail gas in polycrystalline reduction production according to claim 1, it is characterized in that, in described step (2), described in the composition of sorbent material used when adsorbing comprise: the gac of the silica gel of mass percent of 20% ~ 60%, the aluminum oxide of the mass percent of 10% ~ 30% and the mass percent of 10% ~ 70%.
5. polycrystalline reduction according to claim 1 produce in tail gas in the recovery method of dichlorosilane, it is characterized in that, in described step (3), described in carry out one-level rectifying pressure be 0.4 ~ 0.5MPa.
6. polycrystalline reduction according to claim 1 produce in tail gas in the recovery method of dichlorosilane, it is characterized in that, in described step (4), described in carry out two-stage rectification pressure be 0.4 ~ 0.5MPa.
7. a retrieving arrangement for the dichlorosilane in the tail gas in polycrystalline reduction production, is characterized in that, comprising:
Analytic Tower, carries out parsings separation for the tail gas in polycrystalline reduction being produced, obtains the hydrogenchloride separated and chlorosilane;
Adsorption column, is connected with described Analytic Tower, and described adsorption column is used for adsorbing to described chlorosilane the impurity removed containing boron phosphorus;
One-level rectifying tower, is connected with described adsorption column, and described one-level rectifying tower is used for carrying out one-level rectifying and removes light constituent;
Two-stage rectification tower, is connected with described one-level rectifying tower, and described two-stage rectification tower is used for carrying out two-stage rectification and removes heavy constituent, obtains dichlorosilane.
8. the retrieving arrangement of the dichlorosilane in the tail gas in polycrystalline reduction production according to claim 7, it is characterized in that, temperature when resolving in described Analytic Tower is-50 ~ 160 DEG C, and pressure is 0.5 ~ 1.2MPa.
9. the retrieving arrangement of the dichlorosilane in the tail gas in polycrystalline reduction production according to claim 7, it is characterized in that, the temperature of the tower top of described Analytic Tower is-30 ~-10 DEG C.
10. the retrieving arrangement of the dichlorosilane in the tail gas in polycrystalline reduction production according to claim 7, it is characterized in that, the composition of the sorbent material in described adsorption column comprises: the gac of the silica gel of mass percent of 20% ~ 60%, the aluminum oxide of the mass percent of 10% ~ 30% and the mass percent of 10% ~ 70%.
11. polycrystalline reduction according to claim 7 produce in tail gas in the retrieving arrangement of dichlorosilane, it is characterized in that, pressure when described one-level rectifying tower carries out rectifying is 0.4 ~ 0.5MPa.
12. polycrystalline reduction according to claim 7 produce in tail gas in the retrieving arrangement of dichlorosilane, it is characterized in that, pressure when described two-stage rectification tower carries out rectifying is 0.4 ~ 0.5MPa.
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| 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 |
| 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 |
| CN111036029A (en) * | 2018-10-15 | 2020-04-21 | 新特能源股份有限公司 | Method for recovering waste gas in polycrystalline silicon production process |
| 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 |
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| 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 |
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| 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 |
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