CN104003401A - Continuous operative purification system for trichlorosilane - Google Patents

Continuous operative purification system for trichlorosilane Download PDF

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CN104003401A
CN104003401A CN201410240803.4A CN201410240803A CN104003401A CN 104003401 A CN104003401 A CN 104003401A CN 201410240803 A CN201410240803 A CN 201410240803A CN 104003401 A CN104003401 A CN 104003401A
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trichlorosilane
purification
tower group
thick liquid
purification tower
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CN104003401B (en
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姜利霞
严大洲
杨永亮
肖荣晖
汤传斌
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China ENFI Engineering Corp
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China ENFI Engineering Corp
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Abstract

The invention discloses a continuous operative purification system for trichlorosilane. The purification system comprises a purification tower group and a degassing device, wherein the degassing device is arranged on the upstream of the purification tower group along the flowing direction of materials and is used for removing noncondensable gas in a crude trichlorosilane solution; the degassing device comprises a heating system and an exhaust tank; the heating system is arranged on the upstream of the purification tower group along the flowing direction of the materials; and the exhaust tank is arranged between the heating system and the purification tower group and is provided with a noncondensable gas exhaust port. The purification system can be used for heating the crude trichlorosilane solution because the upstream of the purification tower group is provided with the heating system, so that the solubility of the noncondensable gas in the crude trichlorosilane solution is reduced, and furthermore, the noncondensable gas in the crude trichlorosilane solution can be favorably separated and exhausted through the exhaust tank. Therefore, the operating pressure fluctuation generated by the noncondensable gas in the purification tower group in the later period is favorably reduced, and the operating stability of the purification tower group is improved.

Description

The purification system of continuous operating trichlorosilane
Technical field
The present invention relates to field of polysilicon production, in particular to a kind of purification system of continuous operating trichlorosilane.
Background technology
Polysilicon is the base mateiral of manufacturing semiconducter device, unicircuit, solar cell material, is the foundation stone of information and energy industry, is also that country encourages the strategic material of first developing.Most polysilicon makes by improved Siemens in the world at present.Wherein, improved Siemens mainly comprise that trichlorosilane is synthetic, rectification and purification, reduction, tail gas recycle and hydrogenation five processes.Wherein, the principal reaction formula of hydrogenation is as follows:
3SiCl 4+Si+2H 2=4SiHCl 3
The synthetic principal reaction formula of trichlorosilane is as follows:
Si+3HCl=SiHCl 3+H 2
In above-mentioned improved Siemens, rectification and purification operation is the important procedure that guarantees polysilicon purity.Existing rectification and purification operation be by the thick liquid of trichlorosilane of hydrogenation process or synthesis procedure output by comprising the purification tower group of a plurality of rectifying tower, through condensation and vaporization repeatedly, purify.Yet, owing to containing hydrogen or hydrogenchloride in reaction raw materials or product, make inevitably to contain the non-condensable gases such as hydrogen, hydrogenchloride in the thick liquid of trichlorosilane.The existence of these non-condensable gases, can cause the pressure surge in purification tower group on the one hand, affects the pressure environment in purification tower group, causes the operation of purification tower group to produce wild effect, on the other hand, also can increase the burden of later stage tail condenser and tail gas eluting column.
For these reasons, be necessary to propose a kind of effective means, in order to improve purification tower group because of the problem of the fluctuation of service of non-condensable gas generation.
Summary of the invention
The present invention aims to provide a kind of purification system of continuous operating trichlorosilane, to solve the problem of the purification tower group fluctuation of service being caused because of existing of non-condensable gas.
To achieve these goals, according to an aspect of the present invention, a kind of purification system of continuous operating trichlorosilane is provided, comprise purification tower group, also comprise according to the flow direction of material and be arranged on purification tower group upstream, for removing the de-gassing vessel of the thick liquid non-condensable gas of trichlorosilane, de-gassing vessel comprises: heating system and exhaust tank, wherein, heating system is arranged on purification tower group upstream according to the flow direction of material; Exhaust tank is arranged between heating system and purification tower group, and on exhaust tank, is provided with non-condensable gas venting port.
Further, in above-mentioned exhaust tank, be provided with pressure regulating part.
Further, said heating system comprises a plurality of well heaters, and the Heating temperature of each well heater raises successively along the flow direction of material.
Further, said heating system comprises primary heater and the secondary heater setting gradually according to the flow direction of material.
Further, above-mentioned primary heater is interchanger.
Further, in above-mentioned interchanger, thermal medium is the silicon tetrachloride liquid that in purification tower group, weight-removing column flows out.
Further, the weight-removing column with silicon tetrachloride liquid relief outlet is arranged in purification tower group as the first rectifying tower, and the discharge port of exhaust tank is connected with the opening for feed of the first rectifying tower.
Further, also comprise withdrawing can, withdrawing can is connected with the thermal medium outlet of interchanger.
Further, between the thermal medium outlet of withdrawing can and interchanger, be also provided with cooling system.
Apply the purification system of continuous operating trichlorosilane of the present invention.By the heating system arranging in purification tower group upstream, with to carrying out heat treated from hydrogenation process or the thick liquid of synthesis procedure trichlorosilane out.The solubleness of non-condensable gas in the thick liquid of trichlorosilane of heat treated is declined, and then be conducive to make the non-condensable gas being originally dissolved in thick liquid to be separated.And by heating system downstream, exhaust tank being set, when completing the object of discharging non-condensable gas, trichlorosilane can be delivered in purification tower group by thick liquid continuously.In the thick liquid of trichlorosilane of above-mentioned processing, the content of non-condensable gas declines greatly, and this is just conducive to improve the fluctuation that the operating pressure in later stage purification tower group occurs because of non-condensable gas, improves the operation stability of purification tower group.
Accompanying drawing explanation
The Figure of description that forms the application's a part is used to provide a further understanding of the present invention, and schematic description and description of the present invention is used for explaining the present invention, does not form inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 shows according to the purification system of the trichlorosilane of one embodiment of the present invention;
Fig. 2 shows according to the purification system of the trichlorosilane of another embodiment of the present invention;
Fig. 3 shows the de-gassing vessel in the purification system that adopts trichlorosilane in the embodiment of the present invention 1, and in the thick liquid that the thick liquid of trichlorosilane is carried out obtaining after degassed processing, the clearance of non-condensable gas is with the variation diagram of the original content of non-condensable gas;
Fig. 4 shows the de-gassing vessel in the purification system that adopts trichlorosilane in the embodiment of the present invention 2, and in the thick liquid that the thick liquid of trichlorosilane is carried out obtaining after degassed processing, the clearance of non-condensable gas is with the variation diagram of the original content of non-condensable gas;
Fig. 5 shows the de-gassing vessel in the purification system that adopts trichlorosilane in the embodiment of the present invention 3, and in the thick liquid that the thick liquid of trichlorosilane is carried out obtaining after degassed processing, the clearance of non-condensable gas is with the variation diagram of the original content of non-condensable gas;
Fig. 6 shows the de-gassing vessel in the purification system that adopts trichlorosilane in the embodiment of the present invention 4, and in the thick liquid that the thick liquid of trichlorosilane is carried out obtaining after degassed processing, the clearance of non-condensable gas is with the variation diagram of the original content of non-condensable gas;
Fig. 7 shows the de-gassing vessel in the purification system that adopts trichlorosilane in the embodiment of the present invention 5, and in the thick liquid that the thick liquid of trichlorosilane is carried out obtaining after degassed processing, the clearance of non-condensable gas is with the variation diagram of the original content of non-condensable gas; And
Fig. 8 shows the de-gassing vessel in the purification system that adopts trichlorosilane in the embodiment of the present invention 6, and in the thick liquid that the thick liquid of trichlorosilane is carried out obtaining after degassed processing, the clearance of non-condensable gas is with the variation diagram of the original content of non-condensable gas.
Embodiment
It should be noted that, in the situation that not conflicting, embodiment and the feature in embodiment in the application can combine mutually.Describe below with reference to the accompanying drawings and in conjunction with the embodiments the present invention in detail.
As background technology part, introduce, existing trichlorosilane purifying column group has the defect of the fluctuation of service that the existence because of non-condensable gas causes.In order to address this problem, the present inventor provides a kind of purification system of continuous operating trichlorosilane, comprise purification tower group 200, as shown in Figure 1, also comprise according to the flow direction of material and be arranged on purification tower group 200 upstreams, for removing the de-gassing vessel 100 of the thick liquid non-condensable gas of trichlorosilane; De-gassing vessel 100 comprises heating system 110 and exhaust tank 120; Wherein heating system 110 is arranged on purification tower group 200 upstreams according to the flow direction of material, and exhaust tank 120 is arranged between heating system 110 and purification tower group 200, and on exhaust tank 120, is provided with non-condensable gas venting port 121.
The purification system that the present invention is above-mentioned, by the heating system 110 arranging in purification tower group 200 upstreams, with to carrying out heat treated from hydrogenation process or the thick liquid of synthesis procedure trichlorosilane out.The solubleness of non-condensable gas in the thick liquid of trichlorosilane of heat treated is declined, and then be conducive to make the non-condensable gas being originally dissolved in thick liquid to be separated.And by heating system 110 downstreams, exhaust tank 120 being set, when completing the object of discharging non-condensable gas, trichlorosilane can be delivered in purification tower group 200 by thick liquid continuously.In the thick liquid of trichlorosilane of above-mentioned processing, the content of non-condensable gas declines greatly, and this is just conducive to improve the fluctuation that the operating pressure in later stage purification tower group occurs because of non-condensable gas, improves the operation stability of purification tower group.
In the purification system of above-mentioned continuous operating trichlorosilane, under the heat effect of heating system 110, just can make the non-condensable gas in the thick liquid of trichlorosilane be separated.A kind of preferred embodiment in, pressure regulating part is further set in exhaust tank 120.The setting of this pressure regulating part can be adjusted the pressure of exhaust tank inside, and then the thick liquid of trichlorosilane after heating is carried out to step-down processing.By reducing the mode of pressure, further reduce the solubleness of non-condensable gas in the thick liquid of trichlorosilane, and then be more conducive to deviating from of non-condensable gas.
In the process of actually operating, as long as above-mentioned adopted heating system 110 can heat above-mentioned thick liquid.A kind of preferred embodiment in, said heating system 110 comprises a plurality of well heaters, and the Heating temperature of each well heater raises successively along the flow direction of material.This mode heating up gradually has the effect that promotes thick liquid heating rate.For the consideration of heating rate and production cost, those skilled in the art can select concrete well heater kind and number.
Above-mentioned purification tower group 200 generally includes a plurality of weight-removing columns and a plurality of lightness-removing column, and when the thick liquid of trichlorosilane enters after first weight-removing column, the silicon tetrachloride high boiling material in thick liquid can be remained in the below tower reactor of weight-removing column.A kind of preferred embodiment in, heating system 100 comprise according to the flow direction of material, set gradually primary heater and secondary heater.As shown in Figure 2, preferably primary heater is interchanger 111.More preferably, in interchanger 111, thermal medium is the silicon tetrachloride liquid that in purification tower group, weight-removing column flows out.In addition, secondary heater is electric heater 112, and secondary heater can be also the well heater of other types.When the purification system of continuous operating trichlorosilane is set to said structure, the temperature of take in weight-removing column tower reactor is higher (when weight-removing column top is pressed as 0.6MPa, tower reactor temperature is 130 ℃ of left and right) silicon tetrachloride liquid serve as thermal medium, to the thick liquid of trichlorosilane, provide thermal source to carry out preheating, in the thick liquid temp of rising trichlorosilane, can also reduce the temperature of silicon tetrachloride liquid, and then realize heat and exchange, reduce energy consumption effect.
In the process of actually operating, preferably the above-mentioned weight-removing column with silicon tetrachloride liquid relief outlet 211 is arranged in purification tower group 200 as the first rectifying tower 210.Now, the discharge port 122 of exhaust tank 120 and the opening for feed 212 of the first rectifying tower 210 are connected.Above-mentioned being provided with is beneficial to the length that shortens the pipeline of carrying silicon tetrachloride liquid, saves production cost.
In the purification system of above-mentioned continuous operating trichlorosilane, the silicon tetrachloride liquid that exports out from interchanger 111 thermal mediums, can directly enter withdrawing can 310 and recycle.A kind of preferred embodiment in, between the thermal medium outlet of withdrawing can 310 and interchanger 111, be also provided with cooling system 320.By cooling system 320, be conducive to make hot silicon tetrachloride to be cooled to rapidly room temperature, enter subsequently recovery process and again utilize.
According to a further aspect in the invention, also provide the above-mentioned purifying plant purify trichlorosilane of a kind of application method, it comprises the following steps: the thick liquid of trichlorosilane is heated by heating system, be heated to preset temperature; The thick liquid of trichlorosilane after heating is passed into exhaust tank, deviate from non-condensable gas; The thick liquid of the trichlorosilane of deviating from non-condensable gas is passed into purification tower group and purify, obtain trichlorosilane products; Wherein, preset temperature is less than or equal to the temperature of saturation under the first rectifying tower feed plate pressure of described purification tower group.
Term " temperature of saturation " refers to the temperature that liquid and steam have when dynamic balance state (state of saturation) in the present invention.Under different pressures, liquid has different temperature of saturation.Term " temperature of saturation under the first rectifying tower feed plate pressure of purification tower group " refers to: corresponding to the temperature of saturation of the thick liquid of trichlorosilane under the first rectifying tower feed plate pressure of purification tower group.
Aforesaid method provided by the present invention is by heating the thick liquid of trichlorosilane, and the mode of deviating from non-condensable gas reduces non-condensable gas in the thick liquid of trichlorosilane, and the thick liquid of the trichlorosilane of deviating from non-condensable gas is delivered to purification tower group, to improve existing because of non-condensable gas, impact on the operating pressure in purification tower group, and then the operation that improves purification tower group produces wild effect.
In the actually operating of aforesaid method, regard to " liquid in temperature of saturation, in the situation that pressure reduces suddenly, can make partially liq wherein that the problem of vaporizing occurs ".The thick liquid of trichlorosilane is heated to be less than or equal in heating steps of the present invention " temperature of saturation under the first rectifying tower feed plate pressure of purification tower group ".Be heated to this temperature, can be when thick liquid be heated up, reduce non-condensable gas solubleness, prevent that thick liquid from entering the tower stage because the unexpected reduction of pressure makes partially liq that the problem of vaporization occur in the later stage.Thereby be conducive to make non-condensable gas removal and the purification step of the thick liquid of trichlorosilane to be carried out continuously.Preferably, preset temperature is set to equal the temperature of saturation under the first rectifying tower feed plate pressure of purification tower group, is conducive to guarantee that thick liquid smoothly under the prerequisite of charging, makes thick liquid place for high as far as possible state, to improve the rate of discharge of non-condensable gas.
More preferably, the pressure in adjustment exhaust tank is to predetermined pressure, and this predetermined pressure is greater than the first rectifying tower feed plate pressure of purification tower group.Pressure in pressure-pot is set to be greater than " the first rectifying tower feed plate pressure of purification tower group ", also be conducive to prevent that the thick liquid of trichlorosilane from entering after exhaust tank because pressure reduces suddenly partially liq is vaporized, also help the thick liquid of the trichlorosilane making in exhaust tank simultaneously and under the effect of pressure difference, automatically enter purification tower group.
From hydrogenation process or the thick liquid of synthesis procedure trichlorosilane out, be generally the highly pressurised liquid (pressure is generally 2.5Mpa left and right) room temperature, and the first rectifying tower feed plate pressure of purification tower group is usually less than the pressure of the thick liquid of this trichlorosilane.When high pressure raw liquid directly passes into lower pressure column group, near feed plate, can produce certain fluctuation.And the thick liquid of trichlorosilane is carried out to step-down processing by pressure-pot, except can reduce non-condensable gas in thick liquid solubleness, non-condensable gas is discharged, simultaneously, also help and prevent that high pressure raw liquid from directly entering the problem of the caused tower internal pressure fluctuation of purification tower group, is particularly advantageous near the column plate preventing feed plate and occurs unsettled phenomenon.In addition,, because the component ratio of the thick liquid of trichlorosilane out in hydrogenation process or synthesis procedure is non-constant, the thick liquid that while producing continuously, component differs enters purification tower group also can cause the fluctuation of pressure in tower group.And thick liquid is passed into after exhaust tank, storage stops in process, being conducive to make the component ratio homogenization in thick liquid, thereby further improves the operation stability of purification tower group.
In above-mentioned method of purification, to preset temperature, make it enter that exhaust tank reduces pressure and exhaust can reduce the content of non-condensable gas greatly the thick liquid direct heating of trichlorosilane.A kind of preferred embodiment in, the thick liquid of trichlorosilane is heated to preset temperature gradually by a plurality of well heaters.By the thick liquid of trichlorosilane by heating for multiple times to preset temperature, be conducive to improve the intensification efficiency of thick liquid and the continuity of purification process.
In actual operating process, in the step that the thick liquid of trichlorosilane is heated, first silicon tetrachloride liquid weight-removing column in purification tower group being flowed out, as thermal medium, is carried out heat exchange intensification to the thick liquid of trichlorosilane in interchanger, and then by follow-up heater heats to preset temperature.The preheating heat medium of being used as the thick liquid of trichlorosilane from the silicon tetrachloride of the weight-removing column sidepiece below extraction of purification tower group is used, and is conducive to realize heat matched swaps, thereby is conducive to save the production energy consumption of trichlorosilane.More preferably, the weight-removing column with silicon tetrachloride liquid relief outlet is arranged in purification tower group as the first rectifying tower, relies on pressure reduction that the thick liquid of the trichlorosilane of deviating from non-condensable gas in exhaust tank is passed into the first rectifying tower.
The above-mentioned instruction according to the present invention, those skilled in the art have the ability according to the concrete exhaust tank pressure of the first rectifying tower feed plate pressure selection of purification tower group.The thick liquid of trichlorosilane in pressure-pot is passed in the process of purification tower group, also can adopt rare gas element (nitrogen etc.) that thick hydraulic pressure is entered in tower group.A kind of preferred embodiment in, the first rectifying tower feed plate pressure of above-mentioned purification tower group is 0.25~0.6Mpa, the high 0.2~0.9Mpa of the first rectifying tower feed plate pressure of the pressure ratio purification tower group in exhaust tank.Pressure (2.5Mpa left and right) than the thick liquid of trichlorosilane out in hydrogenation process or synthesis procedure, the pressure of exhaust tank is arranged on to above-mentioned scope, be conducive to make the non-condensable gas in thick liquid to be separated out because solubleness under low pressure reduces, be conducive to make the thick liquid in pressure-pot automatically to enter in purification tower group under pressure reduction simultaneously.
Below in conjunction with specific embodiment, the present invention is described in further detail, these embodiment can not be interpreted as restriction the present invention scope required for protection.
For the clearance of non-condensable gas in the thick liquid of trichlorosilane is contrasted, unified the first rectifying tower feed plate pressure of setting the purification tower group adopting in each embodiment is 0.6Mpa, and under this pressure, the temperature of saturation of the thick liquid of trichlorosilane is 110~115 ℃.
Comparative example 1
The thick liquid of trichlorosilane that is 0.01~0.19wt% by non-condensable gas content out in synthesis procedure is heated to 130 ℃, subsequently the thick liquid of 130 ℃ is passed in the pressure-pot of 0.8Mpa, open venting port and carry out after exhaust, when the thick liquid of trichlorosilane is passed into purification tower group, Partial Liquid Phase is vaporized.Making tower charging is gas-liquid mixture or gas phase, and column internals design is according to liquid phase feeding design, causes the interior rectifying section of tower and stripping section gas-liquid load larger with design difference, occurs normally moving tower fluctuation, affects quality product.
Embodiment 1
By pressure out in hydrogenation process, be that 2.5Mpa, non-condensable gas content 19 kinds of thick liquid of trichlorosilane within the scope of 0.01~0.19wt% are heated to respectively 25 ℃, respectively the thick liquid of 25 ℃ is passed in the pressure-pot of 1Mpa subsequently, opening venting port carries out after exhaust, measure the clearance of non-condensable gas in thick liquid, (X-coordinate represents the proper mass content of non-condensable gas in the thick liquid of trichlorosilane to result as shown in Figure 3, ordinate zou is the extrusion rate of non-condensable gas, and unit is %):
When the thick liquid of trichlorosilane after processing passes into purification tower group, charging is smooth.
Embodiment 2
The thick liquid of trichlorosilane that is 0.01~0.19wt% by non-condensable gas content out in synthesis procedure is heated to 70 ℃, subsequently the thick liquid of 70 ℃ is passed in the pressure-pot of 1Mpa, opening venting port carries out after exhaust, measure the clearance of non-condensable gas in thick liquid, (X-coordinate represents the proper mass content of non-condensable gas in the thick liquid of trichlorosilane to result as shown in Figure 4, ordinate zou is the extrusion rate of non-condensable gas, and unit is %):
When the thick liquid of trichlorosilane after processing passes into purification tower group, charging is smooth.
Embodiment 3
The thick liquid of trichlorosilane that is 0.01~0.19wt% by non-condensable gas content out in synthesis procedure is heated to 70 ℃, subsequently the thick liquid of 70 ℃ is passed in the pressure-pot of 1.5Mpa, opening venting port carries out after exhaust, measure the clearance of non-condensable gas in thick liquid, (X-coordinate represents the proper mass content of non-condensable gas in the thick liquid of trichlorosilane to result as shown in Figure 5, ordinate zou is the extrusion rate of non-condensable gas, and unit is %):
When the thick liquid of trichlorosilane after processing passes into purification tower group, charging is smooth.
Embodiment 4
The thick liquid of trichlorosilane that is 0.01~0.19wt% by non-condensable gas content out in synthesis procedure is heated to 70 ℃, subsequently the thick liquid of 70 ℃ is passed in the pressure-pot of 0.8Mpa, opening venting port carries out after exhaust, measure the clearance of non-condensable gas in thick liquid, (X-coordinate represents the proper mass content of non-condensable gas in the thick liquid of trichlorosilane to result as shown in Figure 6, ordinate zou is the extrusion rate of non-condensable gas, and unit is %):
When the thick liquid of trichlorosilane after processing passes into purification tower group, charging is smooth.
Embodiment 5
The thick liquid of trichlorosilane that is 0.01~0.19wt% by non-condensable gas content out in synthesis procedure is heated to 110 ℃, subsequently the thick liquid of 110 ℃ is passed in the pressure-pot of 1Mpa, opening venting port carries out after exhaust, measure the clearance of non-condensable gas in thick liquid, (X-coordinate represents the proper mass content of non-condensable gas in the thick liquid of trichlorosilane to result as shown in Figure 7, ordinate zou is the extrusion rate of non-condensable gas, and unit is %):
When the thick liquid of trichlorosilane after processing passes into purification tower group, charging is smooth.
Embodiment 6
The thick liquid of trichlorosilane that is 0.01~0.19wt% by non-condensable gas content out in synthesis procedure is heated to 110 ℃, subsequently the thick liquid of 110 ℃ is passed in the pressure-pot of 0.8Mpa, opening venting port carries out after exhaust, measure the clearance of non-condensable gas in thick liquid, (X-coordinate represents the proper mass content of non-condensable gas in the thick liquid of trichlorosilane to result as shown in Figure 8, ordinate zou is the extrusion rate of non-condensable gas, and unit is %):
When the thick liquid of trichlorosilane after processing passes into purification tower group, charging is smooth.
From above data with describing, can find out, the above embodiments of the present invention have realized following technique effect: before entering purification tower group, the thick liquid of trichlorosilane is heated up and/or step-down processing, all can effectively remove the non-condensable gas in thick liquid, make the later stage purification tower group can steady running.More especially, for hydrogenchloride non-condensable gas, the original content of hydrogenchloride is higher, and after non-condensable gas is deviate from, the extrusion rate of non-condensable gas is higher.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.

Claims (9)

1. the purification system of a continuous operating trichlorosilane, comprise purification tower group (200), it is characterized in that, also comprise according to the flow direction of material and be arranged on described purification tower group (200) upstream, for removing the de-gassing vessel (100) of the thick liquid non-condensable gas of trichlorosilane, described de-gassing vessel (100) comprising:
Heating system (110), is arranged on described purification tower group (200) upstream according to the flow direction of material;
Exhaust tank (120), is arranged between described heating system (110) and described purification tower group (200), and on described exhaust tank (120), is provided with non-condensable gas venting port (121).
2. purification system according to claim 1, is characterized in that, described exhaust tank is provided with pressure regulating part in (120).
3. purification system according to claim 1 and 2, is characterized in that, described heating system (110) comprises a plurality of well heaters, and the Heating temperature of each well heater raises successively along the flow direction of material.
4. purification system according to claim 3, is characterized in that, described heating system (110) comprises primary heater and the secondary heater setting gradually according to the flow direction of material.
5. purification system according to claim 4, is characterized in that, described primary heater is interchanger (111).
6. purification system according to claim 5, is characterized in that, in described interchanger (111), thermal medium is the silicon tetrachloride liquid that in described purification tower group (200), weight-removing column flows out.
7. according to the purification system described in any one in claim 1 to 6, it is characterized in that, the weight-removing column with silicon tetrachloride liquid relief outlet (211) is arranged in described purification tower group (200) as the first rectifying tower (210), and the discharge port (122) of described exhaust tank (120) is connected with the opening for feed (212) of described the first rectifying tower (210).
8. purification system according to claim 7, is characterized in that, also comprises withdrawing can (310), and described withdrawing can (310) is connected with the thermal medium outlet of described interchanger (111).
9. purification system according to claim 8, is characterized in that, between the thermal medium outlet of described withdrawing can (310) and described interchanger (111), is also provided with cooling system (320).
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CN109748769A (en) * 2017-11-01 2019-05-14 中国石油化工股份有限公司 Butene recovery method during production epoxy butane
CN115594184A (en) * 2022-10-31 2023-01-13 唐山三孚硅业股份有限公司(Cn) Electronic grade silicon tetrachloride production system and method

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CN102471074A (en) * 2009-12-28 2012-05-23 Lg化学株式会社 Method and apparatus for purification of trichlorosilane

Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN109748769A (en) * 2017-11-01 2019-05-14 中国石油化工股份有限公司 Butene recovery method during production epoxy butane
CN115594184A (en) * 2022-10-31 2023-01-13 唐山三孚硅业股份有限公司(Cn) Electronic grade silicon tetrachloride production system and method
CN115594184B (en) * 2022-10-31 2023-10-10 唐山三孚硅业股份有限公司 Electronic grade silicon tetrachloride production system and method

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