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CN105366681B - 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 - Google Patents

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 Download PDF

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CN105366681B
CN105366681B CN201410443572.7A CN201410443572A CN105366681B CN 105366681 B CN105366681 B CN 105366681B CN 201410443572 A CN201410443572 A CN 201410443572A CN 105366681 B CN105366681 B CN 105366681B
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chlorosilane
tower
level
polysilicon
rectifying
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CN105366681A (en
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陈莉娜
宋高杰
张旭
江庆云
其他发明人请求不公开姓名
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Xinte Energy Co Ltd
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Abstract

The invention discloses the processing method of the processing method and system, the also chlorosilane of original production polysilicon recovery of the chlorosilane in a kind for the treatment of method and apparatus of the chlorosilane of also original production polysilicon recovery, production of polysilicon, comprise the following steps:(1) chlorosilane by the also original production polysilicon recovery in production of polysilicon passes through one-level rectifying, then by two-stage rectification, wherein, one-level distillation process obtains silicon tetrachloride, and two-stage rectification process obtains dichlorosilane;(2) dichlorosilane that the silicon tetrachloride and two-stage rectification process obtained one-level distillation process obtains passes through the first anti-disproportionated reaction, obtains trichlorosilane.The chlorosilane dichlorosilane isolated of also original production polysilicon recovery and the silicon tetrachloride separated directly are passed through the first anti-disproportionated reaction by this method, obtain refined trichlorosilane, the refined trichlorosilane need not pass through 5~6 grades of rectification and purification again, it can be directly used for producing polysilicon, energy consumption is reduced, alleviates rectifying load.

Description

The also treating method and apparatus of the chlorosilane of original production polysilicon recovery, polysilicon life The processing method and system of chlorosilane in production
Technical field
The invention belongs to technical field of polysilicon production, and in particular to a kind of chlorosilane of also original production polysilicon recovery The processing method and system of chlorosilane in treating method and apparatus, production of polysilicon.
Background technology
In production of polysilicon, the main source of chlorosilane is the chlorosilane that cold hydrogenation synthesis obtains and also original production polycrystalline The chlorosilane of silicon recovery.
Cold hydrogenation synthesis in production of polysilicon is occurred at high temperature under high pressure mainly using silica flour, silicon tetrachloride, hydrogen Synthetic reaction prepares trichlorosilane, and along with the generation of accessory substance dichlorosilane, finally gives dichlorosilane, trichlorine hydrogen Silicon and silicon tetrachloride mixture, by condensing and washing, obtain the chlorosilane of liquid.Cold hydrogenation synthesis procedure reaction principle:Si+ 3SiCl4+2H2=4SiHCl3(main reaction);Si+SiCl4+2H2=2SiH2Cl2(side reaction);2SiHCl3=SiCl4+SiH2Cl2 (side reaction).Because the raw silicon in cold hydrogenation synthesis procedure reaction and silicon tetrachloride contain a large amount of metal impurities and nonmetallic miscellaneous Matter, after synthetic reaction occurs, the trichlorosilane and accessory substance dichloro hydrogen silicon, silicon tetrachloride of production are, it is necessary to by topping still, essence Evaporate tower and carry out component separation and step by step rectification and purification, can just be met the refining trichlorosilane of production of polysilicon.
Mainly refining trichlorosilane occurs in reduction furnace with hydrogen for also original production polysilicon in production of polysilicon Reduction reaction produces polysilicon, while obtains tail gas, and the tail gas includes chlorosilane gas, hydrogen and hydrogen chloride, by absorbing After parsing, remove hydrogen and most of hydrogen chloride, condensation obtains the chlorosilane of also original production polysilicon recovery.Also original production polycrystalline Silicon process reaction principle:SiHCl3+H2=Si+3HCl (main reaction);(4SiHCl3=Si+3SiCl4+2H2) (side reaction);Si+ 2HCl=SiH2Cl2(side reaction).Because also original production polysilicon process reaction in raw material be refining trichlorosilane, with it is certain During at high temperature reduction reaction occurs for the hydrogen of proportioning, other impurities, therefore accessory substance dichlorosilane, four are not brought into Silicon chloride is also high-purity material.
In production of polysilicon, the dichloro-dihydro silicon impurities that the cold obtained chlorosilane of hydrogenation synthesis is isolated are more, also primary The dichlorosilane that the chlorosilane of production polysilicon recovery is isolated is then high-purity dichlorosilane.In the prior art, polysilicon Enterprise be largely also original production polysilicon recovery that will be in production of polysilicon the dichlorosilane isolated of chlorosilane with it is cold After the dichlorosilane mixing that the chlorosilane that hydrogenation synthesis obtains is isolated, together into anti-disproportionated reaction tower, while with being passed through Anti- disproportionated reaction occurs to the silicon tetrachloride in anti-disproportionated reaction tower, obtains rough trichlorosilane, the rough trichlorosilane In impurity it is more, rough trichlorosilane can not be directly using, it is necessary to which the trichlorosilane rough to this re-starts rectifying, Refined trichlorosilane can be obtained, meets the needs of production of polysilicon.
The content of the invention
The technical problems to be solved by the invention are for above shortcomings in the prior art, there is provided a kind of also primary The processing method and system of the treating method and apparatus of the chlorosilane of production polysilicon recovery, the chlorosilane in production of polysilicon, also Original production polysilicon recovery chlorosilane processing method directly by also original production polysilicon recovery chlorosilane isolate two Chlorine dihydro silicon and the silicon tetrachloride separated pass through the first anti-disproportionated reaction, obtain refined trichlorosilane, and this refined three Chlorine hydrogen silicon need not pass through 5~6 grades of rectification and purification again, be used directly for producing polysilicon, so as to greatly reduce energy consumption, Alleviate rectifying load.
Technical scheme is to provide a kind of chlorine silicon of also original production polysilicon recovery used by solving present invention problem The processing method of alkane, comprises the following steps:
(1) chlorosilane by the also original production polysilicon recovery in production of polysilicon passes through one-level rectifying, then by two level Rectifying, wherein, the one-level distillation process obtains silicon tetrachloride, and the two-stage rectification process obtains dichlorosilane;
(2) dichlorosilane that the silicon tetrachloride and the two-stage rectification process obtained the one-level distillation process obtains By the first anti-disproportionated reaction, trichlorosilane is obtained.
Preferably, the pressure of the described first anti-disproportionated reaction is 0.05~0.1MPaG, and temperature is 45~50 DEG C.
The present invention also provides a kind of processing unit of the chlorosilane of also original production polysilicon recovery, including:
The also chlorosilane storage tank of original production polysilicon recovery, the also original production polysilicon for storing in production of polysilicon return The chlorosilane of receipts;
The also rectifying first stage tower of the chlorosilane of original production polysilicon recovery, the chlorine silicon with the also original production polysilicon recovery Alkane storage tank connects, and the rectifying first stage tower of the chlorosilane of the also original production polysilicon recovery is used for the also original production polysilicon and returned The chlorosilane of receipts carries out one-level rectifying, and the tower reactor of the rectifying first stage tower in the chlorosilane of the also original production polysilicon recovery obtains To silicon tetrachloride;
The also rectifying two level tower of the chlorosilane of original production polysilicon recovery, the chlorine silicon with the also original production polysilicon recovery The tower top of the rectifying first stage tower of alkane connects, and the rectifying two level tower of the chlorosilane of the also original production polysilicon recovery is used for described go back The chlorosilane of original production polysilicon recovery carries out two-stage rectification, and the rectifying of the chlorosilane in the also original production polysilicon recovery The tower top of two level tower obtains dichlorosilane;
First anti-disproportionated reaction tower, the rectifying one with the chlorosilane of the also original production polysilicon recovery respectively of its charging aperture The tower top connection of the tower reactor of level tower, the also rectifying two level tower for the chlorosilane that original production polysilicon reclaims, the first anti-discrimination Change reaction tower be used for the also original production polysilicon recovery chlorosilane rectifying first stage tower the obtained silicon tetrachloride of tower reactor with The dichlorosilane that the tower top of the rectifying two level tower of the chlorosilane of the also original production polysilicon recovery obtains carries out the first anti-discrimination Change reaction and obtain trichlorosilane.
The present invention also provides a kind of processing method of the chlorosilane in production of polysilicon, including above-mentioned also original production polycrystalline The processing method of the chlorosilane of silicon recovery, in addition to cold hydrogenation synthesize the processing method of obtained chlorosilane, comprise the following steps:
(1) chlorosilane for synthesizing to obtain by the cold hydrogenation in production of polysilicon slightly evaporates by one-level, then is slightly evaporated by two level, Wherein, the two level slightly evaporates process and obtains dichlorosilane;
(2) obtain the chlorosilane of the also original production polysilicon recovery in production of polysilicon by one-level distillation process four The chlorosilane that cold hydrogenation in silicon chloride and the production of polysilicon synthesizes to obtain slightly evaporates the dichloro two that process obtains by two level Hydrogen silicon, by the second anti-disproportionated reaction, obtain trichlorosilane.
Preferably, the pressure of the described second anti-disproportionated reaction is 0.05~0.1MPaG, and temperature is 45~50 DEG C.
The present invention also provides a kind of processing system of the chlorosilane in production of polysilicon, including:Above-mentioned also original production is more The processing unit of the chlorosilane of crystal silicon recovery, in addition to cold hydrogenation synthesize the processing unit of obtained chlorosilane, and the device includes:
The chlorosilane storage tank that cold hydrogenation synthesis obtains, the cold hydrogenation for storing in production of polysilicon synthesize obtained chlorine silicon Alkane;
First stage tower slightly is evaporated, the chlorosilane storage tank obtained with the cold hydrogenation synthesis is connected, and described slightly evaporating first stage tower is used for institute The chlorosilane progress one-level that cold hydrogenation synthesis obtains is stated slightly to evaporate;
Slightly evaporate two level tower, with it is described it is thick evaporate first stage tower and be connected, the thick two level tower that evaporates is used to described cold hydrogenate synthesis and obtain Chlorosilane carry out two level and slightly evaporate, and obtain dichlorosilane in the thick tower top for evaporating two level tower;
Second anti-disproportionated reaction tower, the rectifying first stage tower for the chlorosilane that its charging aperture reclaims with going back original production polysilicon respectively Tower reactor, the thick tower top connection for evaporating two level tower, the second anti-disproportionated reaction tower is used for the also original production polysilicon and returns The silicon tetrachloride that the tower reactor of the rectifying first stage tower of the chlorosilane of receipts obtains obtains dichloro-dihydro with the thick tower top for evaporating two level tower Silicon carries out the second anti-disproportionated reaction and obtains trichlorosilane.
Preferably, described cold hydrogenation, which synthesizes the processing unit of obtained chlorosilane, also includes:
Slightly evaporate three-level tower, with it is described it is thick evaporate two level tower and be connected, the thick three-level tower that evaporates is used to described cold hydrogenate synthesis and obtain Chlorosilane carry out three-level slightly evaporate;
The rectifying first stage tower of chlorosilane that cold hydrogenation synthesis obtains, with it is described it is thick evaporate three-level tower and be connected, the cold hydrogenation conjunction Rectifying first stage tower into obtained chlorosilane is used for the cold chlorosilane progress one-level rectifying for hydrogenating synthesis and obtaining;
The rectifying two level tower for the chlorosilane that cold hydrogenation synthesis obtains, the rectifying of the chlorosilane obtained with the cold hydrogenation synthesis First stage tower connects, and the rectifying two level tower for the chlorosilane that the cold hydrogenation synthesis obtains is used for the chlorine silicon that the cold hydrogenation synthesis obtains Alkane carries out two-stage rectification;
The rectifying three-level tower for the chlorosilane that cold hydrogenation synthesis obtains, the rectifying of the chlorosilane obtained with the cold hydrogenation synthesis Two level tower connects, and the rectifying three-level tower for the chlorosilane that the cold hydrogenation synthesis obtains is used for the chlorine silicon that the cold hydrogenation synthesis obtains Alkane carries out three-level rectifying.
The processing method of the chlorosilane of also original production polysilicon recovery in the present invention also original production polysilicon will directly return The dichlorosilane that the chlorosilane of receipts is isolated passes through the first anti-disproportionated reaction with the silicon tetrachloride separated, and obtains refined Trichlorosilane.Above-mentioned processing method, it is cold to avoid the dichlorosilane that the chlorosilane that also original production polysilicon reclaims is isolated The dichlorosilane pollution that the chlorosilane that hydrogenation synthesis obtains is isolated, is used directly as the raw material of the first anti-disproportionated reaction, Reach more economical and more simple flow purpose.The dichlorosilane isolated due to the chlorosilane of also original production polysilicon recovery It is high-purity with the silicon tetrachloride separated, so the refining trichlorosilane obtained by the first anti-disproportionated reaction is also high Pure, the refined trichlorosilane need not pass through 5~6 grades of rectification and purification again, but directly reach refining trichlorosilane Quality requirement, be used directly for produce polysilicon, so as to greatly reduce energy consumption, alleviate rectifying load.
Brief description of the drawings
Fig. 1 is the structural representation of the processing unit of the chlorosilane of the also original production polysilicon recovery in the embodiment of the present invention 2 Figure;
Fig. 2 is the structural representation of the processing system of the chlorosilane in the production of polysilicon in the embodiment of the present invention 4.
In figure:The chlorosilane storage tank of 1- also original production polysilicon recovery;The 2- also chlorosilanes of original production polysilicon recovery Rectifying first stage tower;The tower top of the 21- also rectifying first stage towers of the chlorosilane of original production polysilicon recovery;22- also original production polysilicons The tower reactor of the rectifying first stage tower of the chlorosilane of recovery;The rectifying two level tower of the 3- also chlorosilanes of original production polysilicon recovery;31- is also The tower top of the rectifying two level tower of the chlorosilane of original production polysilicon recovery;The essence of the 32- also chlorosilanes of original production polysilicon recovery Evaporate the charging aperture of two level tower;The tower reactor of the 33- also rectifying two level towers of the chlorosilane of original production polysilicon recovery;4- first is counter to be disproportionated Reaction tower;The charging aperture of the anti-disproportionated reaction towers of 41- first;The chlorosilane storage tank that the cold hydrogenation synthesis of 5- obtains;6- slightly evaporates first stage tower; 61- slightly evaporates the tower top of first stage tower;62- slightly evaporates the tower reactor of first stage tower;63- slightly evaporates the charging aperture of first stage tower;7- slightly evaporates two level tower; 71- slightly evaporates the tower top of two level tower;72- slightly evaporates the charging aperture of two level tower;73- slightly evaporates the tower reactor of two level tower;Anti- disproportionation is anti-by 8- second Answer tower;The charging aperture of the anti-disproportionated reaction towers of 81- second;The tower top of the anti-disproportionated reaction towers of 82- second;The second anti-disproportionated reactions of 83- The tower reactor of tower;9- slightly evaporates three-level tower;91- slightly evaporates the charging aperture of three-level tower;92- slightly evaporates the tower top of three-level tower;The cold hydrogenation synthesis of 10- The rectifying first stage tower of obtained chlorosilane;The charging aperture of the rectifying first stage tower for the chlorosilane that the cold hydrogenation synthesis of 101- obtains;102- The tower reactor of the rectifying first stage tower for the chlorosilane that cold hydrogenation synthesis obtains;The rectifying two level for the chlorosilane that the cold hydrogenation synthesis of 11- obtains Tower;The charging aperture of the rectifying two level tower for the chlorosilane that the cold hydrogenation synthesis of 111- obtains;The chlorosilane that the cold hydrogenation synthesis of 112- obtains Rectifying two level tower tower top;The rectifying three-level tower for the chlorosilane that the cold hydrogenation synthesis of 12- obtains;The cold hydrogenation synthesis of 121- obtains The charging aperture of the rectifying three-level tower of chlorosilane;The tower reactor of the rectifying three-level tower for the chlorosilane that the cold hydrogenation synthesis of 122- obtains;13- hands Valve.
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 present embodiment provides a kind of processing method of the chlorosilane of also original production polysilicon recovery, comprises the following steps:
(1) chlorosilane by the also original production polysilicon recovery in production of polysilicon passes through one-level rectifying, then by two level Rectifying, wherein, the one-level distillation process obtains silicon tetrachloride, and the two-stage rectification process obtains dichlorosilane;
(2) dichlorosilane that the silicon tetrachloride and the two-stage rectification process obtained the one-level distillation process obtains By the first anti-disproportionated reaction, trichlorosilane is obtained.
Preferably, the pressure of the described first anti-disproportionated reaction is 0.05~0.1MPaG, and temperature is 45~50 DEG C.
In production of polysilicon, the dichloro-dihydro silicon impurities that the cold obtained chlorosilane of hydrogenation synthesis is isolated are more, also primary The dichlorosilane that the chlorosilane of production polysilicon recovery is isolated is then high-purity dichlorosilane.In the prior art, polysilicon Enterprise be largely also original production polysilicon recovery that will be in production of polysilicon the dichlorosilane isolated of chlorosilane with it is cold After the dichlorosilane mixing that the chlorosilane that hydrogenation synthesis obtains is isolated, cold hydrogenation synthesizes obtained chlorosilane is isolated two Chlorine dihydro silicon can pollute the dichlorosilane that the chlorosilane of also original production polysilicon recovery is isolated.What cold hydrogenation synthesis obtained The amount for the dichlorosilane that chlorosilane is isolated is less, as long as but being isolated with the chlorosilane of also original production polysilicon recovery Dichlorosilane mixes, will the dichlorosilane isolated of chlorosilane of pair also original production polysilicon recovery pollute, from And the quality of trichlorosilane made from influenceing, it is necessary to purified again to obtained trichlorosilane.
In the present embodiment, the dichloro two isolated of chlorosilane of also original production polysilicon recovery that will be in production of polysilicon The dichlorosilane that the chlorosilane that hydrogen silicon obtains with cold hydrogenation synthesis is isolated mixes, but also original production polysilicon will directly return The dichlorosilane that the chlorosilane of receipts is isolated passes through the first anti-disproportionated reaction with the silicon tetrachloride separated, and obtains refined Trichlorosilane.Above-mentioned processing method, it is cold to avoid the dichlorosilane that the chlorosilane that also original production polysilicon reclaims is isolated The dichlorosilane pollution that the chlorosilane that hydrogenation synthesis obtains is isolated, is used directly as the raw material of the first anti-disproportionated reaction, Reach more economical and more simple flow purpose.The dichlorosilane isolated due to the chlorosilane of also original production polysilicon recovery It is high-purity with the silicon tetrachloride separated, so the refining trichlorosilane obtained by the first anti-disproportionated reaction is also high Pure, the refined trichlorosilane need not pass through 5~6 grades of rectification and purification again, but directly reach refining trichlorosilane Quality requirement, be used directly for produce polysilicon, so as to greatly reduce energy consumption, alleviate rectifying load.
Embodiment 2
As shown in figure 1, the present embodiment provides a kind of processing unit of the chlorosilane of also original production polysilicon recovery, including:
The also chlorosilane storage tank 1 of original production polysilicon recovery, for storing the also original production polysilicon in production of polysilicon The chlorosilane of recovery;
The also rectifying first stage tower 2 of the chlorosilane of original production polysilicon recovery, the chlorine with the also original production polysilicon recovery Silane storage tank 1 connects, and the rectifying first stage tower 2 of the chlorosilane of the also original production polysilicon recovery is used for the also original production polycrystalline The chlorosilane of silicon recovery carries out one-level rectifying, and in the tower of the also rectifying first stage tower for the chlorosilane that original production polysilicon reclaims Kettle 22 obtains silicon tetrachloride;
The also rectifying two level tower 3 of the chlorosilane of original production polysilicon recovery, the chlorine with the also original production polysilicon recovery The tower top 21 of the rectifying first stage tower of silane connects, and the rectifying two level tower 3 of the chlorosilane of the also original production polysilicon recovery is used for The chlorosilane of the also original production polysilicon recovery carries out two-stage rectification, and in the chlorosilane of the also original production polysilicon recovery The tower top 31 of rectifying two level tower obtain dichlorosilane;
First anti-disproportionated reaction tower 4, the charging aperture 41 of the first anti-disproportionated reaction tower go back original production polysilicon with described respectively The tower reactor 22 of the rectifying first stage tower of the chlorosilane of recovery, the also original production polysilicon recovery chlorosilane rectifying two level tower Tower top 31 connects, and the first anti-disproportionated reaction tower 4 is used for the rectifying one-level of the chlorosilane of the also original production polysilicon recovery The tower top 31 of the silicon tetrachloride that the tower reactor 22 of tower obtains and the rectifying two level tower of the chlorosilane of the also original production polysilicon recovery Obtained dichlorosilane carries out the first anti-disproportionated reaction and obtains trichlorosilane.Specifically, the first anti-disproportionation in the present embodiment Silicon tetrachloride and dichlorosilane are placed with reaction tower 4 can carry out the catalyst of anti-disproportionated reaction.First anti-disproportionated reaction The tower top of tower 4 come out product main component be trichlorosilane, wherein impurity content be P≤10PPb, B≤5PPb, Fe≤ 50PPb, Ca≤80PPb, Al≤80PPb, the product are refined trichlorosilane.
In the present embodiment, the tower top 21 of the rectifying first stage tower of the chlorosilane of specific also original production polysilicon recovery and reduction The charging aperture 32 of the rectifying two level tower of the chlorosilane of production polysilicon recovery connects.In the chlorosilane of also original production polysilicon recovery The tower top 21 of rectifying first stage tower obtain the mixture of dichlorosilane and trichlorosilane, in the chlorine of also original production polysilicon recovery The tower reactor 22 of the rectifying first stage tower of silane arrives silicon tetrachloride.In the also rectifying two level tower of the chlorosilane of original production polysilicon recovery Tower top 31 obtains dichlorosilane, and trichlorine is obtained in the tower reactor 33 of the also rectifying two level tower of the chlorosilane of original production polysilicon recovery Hydrogen silicon.Realize the distillation process of the rectifying first stage tower 2 of the chlorosilane of above-mentioned also original production polysilicon recovery, go back original production polysilicon The distillation process of the rectifying two level tower 3 of the chlorosilane of recovery obtains above-mentioned each component, belongs to what chemical field can be realized.
The processing unit of the chlorosilane of also original production polysilicon recovery in the present embodiment will directly go back original production polysilicon The dichlorosilane that the chlorosilane of recovery is isolated passes through the first anti-disproportionated reaction with the silicon tetrachloride separated, and is refined Trichlorosilane.Above-mentioned processing unit, avoid the dichlorosilane quilt that the chlorosilane of also original production polysilicon recovery is isolated The dichlorosilane pollution that the chlorosilane that cold hydrogenation synthesis obtains is isolated, makes directly as the raw material of the first anti-disproportionated reaction With reaching more economical and more simple flow purpose.The dichloro two isolated due to the chlorosilane of also original production polysilicon recovery Hydrogen silicon and the silicon tetrachloride separated are high-purity, so the refining trichlorosilane obtained by the first anti-disproportionated reaction It is high-purity, the refined trichlorosilane need not pass through 5~6 grades of rectification and purification again, but directly reach refined trichlorine The quality requirement of hydrogen silicon, it is used directly for producing polysilicon, so as to greatly reduce energy consumption, alleviates rectifying load.
Embodiment 3
The present embodiment provides a kind of processing method of the chlorosilane in production of polysilicon, including above-mentioned also original production polycrystalline The processing method of the chlorosilane of silicon recovery, in addition to cold hydrogenation synthesize the processing method of obtained chlorosilane, comprise the following steps:
(1) chlorosilane for synthesizing to obtain by the cold hydrogenation in production of polysilicon slightly evaporates by one-level, then is slightly evaporated by two level, Wherein, the two level slightly evaporates process and obtains dichlorosilane;
(2) obtain the chlorosilane of the also original production polysilicon recovery in production of polysilicon by one-level distillation process four The chlorosilane that cold hydrogenation in silicon chloride and the production of polysilicon synthesizes to obtain slightly evaporates the dichloro two that process obtains by two level Hydrogen silicon, by the second anti-disproportionated reaction, obtain trichlorosilane.
Preferably, the pressure of the described second anti-disproportionated reaction is 0.05~0.1MPaG, and temperature is 45~50 DEG C.
In the present embodiment, the dichloro two isolated of chlorosilane of also original production polysilicon recovery that will be in production of polysilicon The dichlorosilane that the chlorosilane that hydrogen silicon obtains with cold hydrogenation synthesis is isolated mixes, but respectively:Original production polysilicon will be gone back The dichlorosilane that the chlorosilane of recovery is isolated passes through the first anti-disproportionated reaction with the silicon tetrachloride separated, and obtains trichlorine Hydrogen silicon;The dichlorosilane and the chlorosilane point of also original production polysilicon recovery that the chlorosilane that cold hydrogenation synthesis obtains is isolated The silicon tetrachloride separated out passes through the second anti-disproportionated reaction, obtains trichlorosilane.Can be with, while will be also primary in production of polysilicon Produce dichlorosilane, the cold dichloro-dihydro for hydrogenating the chlorosilane that synthesis obtains and isolating that the chlorosilane of polysilicon recovery is isolated Silicon is respectively processed to obtain trichlorosilane, so as to reach the purpose of the processing of the chlorosilane in production of polysilicon.Directly will The also chlorosilane dichlorosilane isolated of original production polysilicon recovery and the silicon tetrachloride separated passes through the first anti-discrimination To change reaction, obtain refined trichlorosilane, the refined trichlorosilane need not pass through 5~6 grades of rectification and purification again, but directly The quality requirement of refining trichlorosilane has been accessed, has been used directly for producing polysilicon, so as to greatly reduce energy consumption, has been mitigated Rectifying load.
Embodiment 4
As shown in Fig. 2 the present embodiment provides a kind of processing system of the chlorosilane in production of polysilicon, including:Above-mentioned The also processing unit of the chlorosilane of original production polysilicon recovery, in addition to cold hydrogenation synthesize the processing unit of obtained chlorosilane, The device includes:
The chlorosilane storage tank 5 that cold hydrogenation synthesis obtains, the cold hydrogenation for storing in production of polysilicon synthesize obtained chlorine Silane;
First stage tower 6 slightly is evaporated, is connected with the cold obtained chlorosilane storage tank 5 of hydrogenation synthesis, it is described thick to evaporate first stage tower 6 and be used for The chlorosilane that the cold hydrogenation synthesis obtains carries out one-level and slightly evaporated;
Slightly evaporate two level tower 7, with it is described it is thick evaporate first stage tower 6 and be connected, it is described it is thick evaporate two level tower 7 and be used for the cold hydrogenation synthesize To chlorosilane carry out two level and slightly evaporate, and obtain dichlorosilane in the thick tower top 71 for evaporating two level tower;
Second anti-disproportionated reaction tower 8, the charging aperture 81 of the second anti-disproportionated reaction tower reclaim with also original production polysilicon respectively The tower reactor 22 of rectifying first stage tower of chlorosilane, the thick tower top 71 for evaporating two level tower connect, the second anti-disproportionated reaction tower 8 For the chlorosilane of the also original production polysilicon recovery rectifying first stage tower the obtained silicon tetrachloride of tower reactor 22 with it is described thick Evaporate two level tower tower top 71 obtain dichlorosilane carry out the second anti-disproportionated reaction obtain trichlorosilane.Specifically, the present embodiment In the second anti-disproportionated reaction tower 8 in be placed with silicon tetrachloride and dichlorosilane and can carry out the catalyst of anti-disproportionated reaction.
Preferably, described cold hydrogenation, which synthesizes the processing unit of obtained chlorosilane, also includes:
Slightly evaporate three-level tower 9, with it is described it is thick evaporate two level tower 7 and be connected, it is described it is thick evaporate three-level tower 9 and be used for the cold hydrogenation synthesize To chlorosilane carry out three-level slightly evaporate;
The rectifying first stage tower 10 of chlorosilane that cold hydrogenation synthesis obtains, with it is described it is thick evaporate three-level tower 9 and be connected, the cold hydrogenation The rectifying first stage tower 10 for synthesizing obtained chlorosilane is used for the chlorosilane progress one-level rectifying that the cold hydrogenation synthesis obtains;
The rectifying two level tower 11 for the chlorosilane that cold hydrogenation synthesis obtains, the essence of the chlorosilane obtained with the cold hydrogenation synthesis Evaporate first stage tower 10 to connect, the rectifying two level tower 11 for the chlorosilane that the cold hydrogenation synthesis obtains is used for the cold hydrogenation synthesis and obtained Chlorosilane carry out two-stage rectification;
The rectifying three-level tower 12 for the chlorosilane that cold hydrogenation synthesis obtains, the essence of the chlorosilane obtained with the cold hydrogenation synthesis Evaporate two level tower 11 to connect, the rectifying three-level tower 12 for the chlorosilane that the cold hydrogenation synthesis obtains is used for the cold hydrogenation synthesis and obtained Chlorosilane carry out three-level rectifying.
In the present embodiment, the tower top 61 for slightly evaporating first stage tower is connected with the charging aperture 72 for slightly evaporating two level tower, slightly evaporates two level tower Tower reactor 73 is connected with slightly evaporating the charging aperture 91 of three-level tower, and the tower top 92 and cold hydrogenation for slightly evaporating three-level tower synthesize obtained chlorosilane The charging aperture 101 of rectifying first stage tower connects, the tower reactor 102 of the rectifying first stage tower for the chlorosilane that cold hydrogenation synthesis obtains and cold hydrogenation The charging aperture 111 for synthesizing the rectifying two level tower of obtained chlorosilane connects, the rectifying two level for the chlorosilane that cold hydrogenation synthesis obtains The charging aperture 121 of the rectifying three-level tower for the chlorosilane that the tower top 112 of tower obtains with cold hydrogenation synthesis is connected.
In the present embodiment, rough heavy constituent silicon tetrachloride is obtained in the tower reactor 62 for slightly evaporating first stage tower, is slightly evaporating first stage tower Tower top 61 obtain the mixture of rough dichlorosilane and rough trichlorosilane.Obtained in the tower reactor 73 for slightly evaporating two level tower Rough trichlorosilane, rough dichlorosilane is obtained in the tower top 71 for slightly evaporating two level tower.The thick tower reactor 73 for evaporating two level tower Rough trichlorosilane is successively by slightly evaporating three-level tower 9, the rectifying first stage tower 10 for the chlorosilane that cold hydrogenation synthesis obtains, cold hydrogenation Synthesize the rectifying two level tower 11 of obtained chlorosilane, the rectifying three-level tower 12 for the chlorosilane that cold hydrogenation synthesis obtains carries out level Four and taken off Light component takes off heavy constituent, and refined trichlorine hydrogen is obtained in the tower reactor 122 of the rectifying three-level tower for the chlorosilane that cold hydrogenation synthesis obtains Silicon.
Due in the prior art, the tower top 31 and second of the rectifying two level tower of the chlorosilane of original production polysilicon recovery will be gone back The charging aperture 81 of anti-disproportionated reaction tower connects, so in the tower of the also rectifying two level tower of the chlorosilane of original production polysilicon recovery The pipeline of material transportation is provided between the charging aperture 81 of 31 and second anti-disproportionated reaction tower of top., only need to be at this in the present embodiment Increase the switch of a control material flow on pipeline, the switch is set to off closed state, by also original production polysilicon The connecting pipeline of the charging aperture 81 of the 31 and second anti-disproportionated reaction tower of tower top of the rectifying two level tower of the chlorosilane of recovery blocks, and leads to Cross this method and simple transformation is done to pipeline of the prior art.In the present embodiment, the switch is specially hand valve 13.
Preferably, the tower top 82 of the described second anti-disproportionated reaction tower is connected with the thick charging aperture 63 for evaporating first stage tower, The tower reactor 83 of the second anti-disproportionated reaction tower obtains trichlorosilane, the liquid that the tower top 82 of the second anti-disproportionated reaction tower obtains Mutually thick trichlorosilane can be passed through thick evaporate and continue one-level in first stage tower 6 and slightly evaporate.
In the present embodiment by slightly evaporate first stage tower 6, it is thick evaporate two level tower 7, it is thick evaporate three-level tower 9, the chlorine that cold hydrogenation synthesis obtains The chlorine silicon that the rectifying two level tower 11 for the chlorosilane that the rectifying first stage tower 10 of silane, cold hydrogenation synthesis obtain, cold hydrogenation synthesis obtain The rectifying three-level tower 12 of alkane, three-level is carried out and has taken off light component and the de- heavy constituent of three-level, light component and heavy constituent have been separated.Relative to For trichlorosilane, dichloro hydrogen silicon, boron chloride, silane etc. belong to light component, silicon tetrachloride, phosphorus trichloride, iron content or aluminium Or metal impurities of calcium etc. belong to heavy constituent.In the present embodiment, slightly evaporate first stage tower 6 and be used to remove heavy constituent silicon tetrachloride, slightly Evaporate two level tower 7 to be used to remove light component dichloro hydrogen silicon, it is miscellaneous slightly to evaporate the heavy constituent that three-level tower 9 is used to remove close to trichlorosilane boiling point Matter, the rectifying first stage tower 10 for the chlorosilane that cold hydrogenation synthesis obtains are used to remove the light component impurity close to trichlorosilane boiling point, The rectifying two level tower 11 for the chlorosilane that cold hydrogenation synthesis obtains is used to remove heavy constituent impurity, the chlorosilane that cold hydrogenation synthesis obtains Rectifying three-level tower 12 be used for remove light component impurity.In the present embodiment, by the way that the thick tower top 71 for evaporating two level tower is obtained Dichlorosilane be passed into the second anti-disproportionated reaction tower 8 and carry out the second anti-disproportionated reaction, so as to greatly reduce cold hydrogenation The load of the front end of the processing unit of obtained chlorosilane is synthesized, energy consumption is reduced, reduces processing cost.
The processing system of the chlorosilane in production of polysilicon in the present embodiment, reduce the chlorine silicon that cold hydrogenation synthesis obtains The thick load evaporated with 3 grades of rectifying of 3 grades of the processing unit of alkane, improve the processing system processing of the chlorosilane in production of polysilicon The ability of chlorosilane, expand the production capacity of refining trichlorosilane.
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 (5)

1. the processing method of the chlorosilane in a kind of production of polysilicon, it is characterised in that including also original production polysilicon recovery The chlorosilane of the processing method, the also recovery of original production polysilicon of the chlorosilane that the processing method of chlorosilane and cold hydrogenation synthesis obtain Processing method comprise the following steps:
(1) chlorosilane of also original production polysilicon recovery that will be in production of polysilicon passes through one-level rectifying, then by two-stage rectification, Wherein, the one-level distillation process obtains silicon tetrachloride, and the two-stage rectification process obtains dichlorosilane;
(2) dichlorosilane that the silicon tetrachloride and the two-stage rectification process obtained the one-level distillation process obtains is passed through First anti-disproportionated reaction, obtains trichlorosilane;
The processing method for the chlorosilane that cold hydrogenation synthesis obtains comprises the following steps:
(1) chlorosilane for synthesizing to obtain by the cold hydrogenation in production of polysilicon slightly evaporates by one-level, then is slightly evaporated by two level, its In, the two level slightly evaporates process and obtains dichlorosilane;
(2) four chlorinations for obtaining the chlorosilane of the also original production polysilicon recovery in production of polysilicon by one-level distillation process The chlorosilane that cold hydrogenation in silicon and the production of polysilicon synthesizes to obtain slightly evaporates the dichlorosilane that process obtains by two level, By the second anti-disproportionated reaction, trichlorosilane is obtained.
2. the processing method of the chlorosilane in production of polysilicon according to claim 1, it is characterised in that described first is anti- The pressure of disproportionated reaction is 0.05~0.1MPaG, and temperature is 45~50 DEG C.
3. the processing method of the chlorosilane in production of polysilicon according to claim 1, it is characterised in that described second is anti- The pressure of disproportionated reaction is 0.05~0.1MPaG, and temperature is 45~50 DEG C.
A kind of 4. processing system of the chlorosilane in production of polysilicon, it is characterised in that including:Also original production polysilicon reclaims The processing unit for the chlorosilane that the processing unit of chlorosilane and cold hydrogenation synthesis obtain,
The processing unit of the chlorosilane of the also original production polysilicon recovery includes:
The also chlorosilane storage tank of original production polysilicon recovery, for storing the also original production polysilicon recovery in production of polysilicon Chlorosilane;
The also rectifying first stage tower of the chlorosilane of original production polysilicon recovery, stored up with the chlorosilane of the also original production polysilicon recovery Tank connects, and the rectifying first stage tower of the chlorosilane of the also original production polysilicon recovery is used for the also original production polysilicon recovery Chlorosilane carries out one-level rectifying, and the tower reactor of the rectifying first stage tower in the chlorosilane of the also original production polysilicon recovery obtains four Silicon chloride;
The also rectifying two level tower of the chlorosilane of original production polysilicon recovery, with the chlorosilane of the also original production polysilicon recovery The tower top connection of rectifying first stage tower, the rectifying two level tower of the chlorosilane of the also original production polysilicon recovery is for described also primary The chlorosilane for producing polysilicon recovery carries out two-stage rectification, and the rectifying two level of the chlorosilane in the also original production polysilicon recovery The tower top of tower obtains dichlorosilane;
First anti-disproportionated reaction tower, its charging aperture respectively with it is described also original production polysilicon recovery chlorosilane rectifying first stage tower Tower reactor, the also original production polysilicon recovery chlorosilane rectifying two level tower tower top connection, the described first anti-disproportionation is anti- Answer tower be used for the also obtained silicon tetrachloride of tower reactor of the rectifying first stage tower for the chlorosilane that original production polysilicon reclaims with it is described The dichlorosilane that the tower top of the also rectifying two level tower of the chlorosilane of original production polysilicon recovery obtains carries out first and is instead disproportionated instead Trichlorosilane should be obtained;
The processing unit for the chlorosilane that the cold hydrogenation synthesis obtains includes:
The chlorosilane storage tank that cold hydrogenation synthesis obtains, the cold hydrogenation for storing in production of polysilicon synthesize obtained chlorosilane;
First stage tower slightly is evaporated, the chlorosilane storage tank obtained with the cold hydrogenation synthesis is connected, and the thick first stage tower that evaporates is for described cold The chlorosilane that hydrogenation synthesis obtains carries out one-level and slightly evaporated;
Slightly evaporate two level tower, with it is described it is thick evaporate first stage tower and be connected, it is described it is thick evaporate two level tower and be used for the cold hydrogenation synthesize obtained chlorine Silane carries out two level and slightly evaporated, and obtains dichlorosilane in the thick tower top for evaporating two level tower;
Second anti-disproportionated reaction tower, the tower of the rectifying first stage tower for the chlorosilane that its charging aperture reclaims with going back original production polysilicon respectively Kettle, the thick tower top connection for evaporating two level tower, the second anti-disproportionated reaction tower are used for the also original production polysilicon recovery The silicon tetrachloride that the tower reactor of the rectifying first stage tower of chlorosilane obtains obtains dichlorosilane with the thick tower top for evaporating two level tower and entered The second anti-disproportionated reaction of row obtains trichlorosilane.
5. the processing system of the chlorosilane in production of polysilicon according to claim 4, it is characterised in that described cold hydrogen The processing unit for the chlorosilane for being combined to obtain also includes:
Slightly evaporate three-level tower, with it is described it is thick evaporate two level tower and be connected, it is described it is thick evaporate three-level tower and be used for the cold hydrogenation synthesize obtained chlorine Silane carries out three-level and slightly evaporated;
The rectifying first stage tower of chlorosilane that cold hydrogenation synthesis obtains, with it is described it is thick evaporate three-level tower and be connected, cold hydrogenate synthesizes To the rectifying first stage tower of chlorosilane be used for the cold obtained chlorosilane of hydrogenation synthesis and carry out one-level rectifying;
The rectifying two level tower for the chlorosilane that cold hydrogenation synthesis obtains, the rectifying one-level of the chlorosilane obtained with the cold hydrogenation synthesis Tower connects, and the rectifying two level tower for the chlorosilane that the cold hydrogenation synthesis obtains is used for the chlorosilane that the cold hydrogenation synthesis obtains and entered Row two-stage rectification;
The rectifying three-level tower for the chlorosilane that cold hydrogenation synthesis obtains, the rectifying two level of the chlorosilane obtained with the cold hydrogenation synthesis Tower connects, and the rectifying three-level tower for the chlorosilane that the cold hydrogenation synthesis obtains is used for the chlorosilane that the cold hydrogenation synthesis obtains and entered Row three-level rectifying.
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