CN107648979A - The method and system of tail gas in a kind of processing production of polysilicon - Google Patents

The method and system of tail gas in a kind of processing production of polysilicon Download PDF

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Publication number
CN107648979A
CN107648979A CN201610592188.2A CN201610592188A CN107648979A CN 107648979 A CN107648979 A CN 107648979A CN 201610592188 A CN201610592188 A CN 201610592188A CN 107648979 A CN107648979 A CN 107648979A
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tail gas
polysilicon
production
adsorbing mechanism
absorption
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相文强
张吉武
侯雨
张凯兴
孙荣义
黄鹏
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Xinte Energy Co Ltd
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Xinte Energy Co Ltd
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Priority to CN201610592188.2A priority Critical patent/CN107648979A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/20Halogens or halogen compounds
    • B01D2257/202Single element halogens
    • B01D2257/2025Chlorine

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention discloses a kind of method and system for handling tail gas in production of polysilicon, this method comprises the following steps:Tail gas in production of polysilicon is adsorbed, dichlorosilane, trichlorosilane in absorption production of polysilicon in tail gas, hydrogen chloride, obtains tail gas in the production of polysilicon after absorption;Adsorbed material is desorbed, obtains tail gas in the production of polysilicon of desorption out, tail gas includes dichlorosilane, trichlorosilane and hydrogen chloride in the production of polysilicon for being desorbed out;Using the silicon tetrachloride containing liquid elution liquid condensing and elute desorption out production of polysilicon in tail gas, tail gas in scrubbed leacheate and scrubbed production of polysilicon is obtained, scrubbed leacheate includes silicon tetrachloride, dichlorosilane, trichlorosilane and hydrogen chloride.The defects of solving effective recovery that existing cryogenic condensation technology can not realize chlorosilane in tail gas, while continuing to reduce condensation temperature increase cooling medium consumption and equipment investment problem.

Description

The method and system of tail gas in a kind of processing production of polysilicon
Technical field
The invention belongs to technical field of polysilicon production, and in particular to it is a kind of handle production of polysilicon in tail gas method and System.
Background technology
With the continuous lifting of China's environmental policy in recent years, domestic polysilicon enterprise is real by continuing to develop and improving The recycling and harmless treatment of most tail gas in polysilicon production process, waste liquid and solid slag are showed.But with Continuous improvement of the market to impurity concentration requirement in polysilicon, for constantly lifting polysilicon product quality, polysilicon production process In certainly will caused by a large amount of acid tail gas.In order to handle this partial tail gas, most enterprises still take the mode that alkali lye elutes Handled, this method had both consumed a large amount of alkali lye, added silicon consumption, chlorine consumption and alkaline consumption in polysilicon production process again.OK Ye Zhongyeyou enterprises handle tail gas and waste liquid in production of polysilicon by the way of burning, but the flow that this mode is handled is answered It is miscellaneous, the chlorosilane in tail gas, waste liquid can not be subjected to recycling, accessory substance belongs to production capacity surplus product in indivedual areas, The increase of the performance of enterprises can not be realized.
Caused tail gas mainly contains N in polysilicon production process2、H2、SiH2Cl2、SiHCl3, HCl etc., wherein big portion absolutely It is divided into N2、H2On-condensible gas, accounting is 80% or so, and remainder is the chlorosilane sour gas that material system is released, composition In mainly contain SiH2Cl2、SiHCl3、HCl.Due to SiH2Cl2、SiHCl3Volatility it is of a relatively high, be easily condensed into liquid phase, can So that caused tail gas in polysilicon production process is condensed and eluted at low temperature using the silicon tetrachloride of liquid, tail is removed Impurity in gas simultaneously absorbs the hydrogen chloride and chlorosilane of part.But because the accounting of the fixed gas in tail gas is higher, gas phase chlorine The condensation effect of silane is poor.In addition, the accounting of gas phase chlorosilane is relatively low in tail gas after elution, and it is not easy to be condensed, So that the pressure that the alkali lye elution device of subsequent technique carries out alkali lye elution processing is still larger, the alkali lye elution dress of subsequent technique The alkali lye consumption amount put is still high.
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 one kind processing is more The method and system of tail gas in crystal silicon production, the effective of chlorosilane in tail gas can not be realized by solving existing cryogenic condensation technology Recovery, while continue to reduce the defects of condensation temperature increases cooling medium consumption and equipment investment problem.
Technical scheme is to provide a kind of side for handling tail gas in production of polysilicon used by solving present invention problem Method, tail gas includes nitrogen, hydrogen, dichlorosilane, trichlorosilane and hydrogen chloride in the production of polysilicon, and methods described includes Following steps:
Tail gas in production of polysilicon is adsorbed, dichlorosilane, trichlorine hydrogen in absorption production of polysilicon in tail gas Silicon, hydrogen chloride, obtain tail gas in the production of polysilicon after absorption, tail gas bag in the production of polysilicon after absorption Include nitrogen and hydrogen;
Adsorbed material is desorbed, obtains tail gas in the production of polysilicon of desorption out, what the desorption came out Tail gas includes dichlorosilane, trichlorosilane and hydrogen chloride in production of polysilicon;
Using the silicon tetrachloride containing liquid elution liquid condensing and elute it is described desorption out production of polysilicon in tail Gas, obtains tail gas in scrubbed leacheate and scrubbed production of polysilicon, and the scrubbed leacheate includes Silicon tetrachloride, dichlorosilane, trichlorosilane and hydrogen chloride.
By handling in production of polysilicon after the method for tail gas, tail gas key component in the production of polysilicon after absorption For nitrogen and hydrogen, can be directly vented after the alkali lye elution of subsequent technique;Tail gas in production of polysilicon after scrubbed Key component is nitrogen and hydrogen, and wherein chlorosilane accounting is 1~5wt%, can be direct after the alkali lye elution of subsequent technique Emptying, scrubbed leacheate are put into recycling after entering the rectifier unit separation of subsequent technique.
Preferably, the adsorption step can also adsorb in production of polysilicon the impurity containing boron, phosphorus in tail gas.
Preferably, the adsorption step is adsorbed using adsorbent, and the adsorbent is modified activated carbon.
Preferably, the temperature of the adsorption step is 0~70 DEG C.
Preferably, the temperature of the desorption is 100~180 DEG C.
Preferably, the temperature of the rinsing step is -40~0 DEG C.Due to after adsorption/desorption so that desorption comes out Production of polysilicon in the content of fixed gas in tail gas substantially reduce, can so greatly improve condensation point so that be desorbed out Tail gas is easier to make for condensing in the production of polysilicon come.The method of the present invention can be carried out under relatively high condensation temperature Elution absorbs the chlorosilane and hydrogen chloride in tail gas in the production of polysilicon for being desorbed out, and realize has to chlorosilane in tail gas Effect recovery, reduce cooling medium consumption and equipment investment.
Preferably, described the step of being desorbed adsorbed material, is specially:Using obtaining after absorption Production of polysilicon in tail gas adsorbed material is desorbed.
Preferably, in described processing production of polysilicon tail gas method, it is further comprising the steps of:
Tail gas in production of polysilicon before adsorbing is carried out being pressurized to 0.1~0.5Mpa.
The present invention also provides a kind of system for handling tail gas in production of polysilicon, and tail gas includes nitrogen in the production of polysilicon Gas, hydrogen, dichlorosilane, trichlorosilane and hydrogen chloride, the system include:
Adsorbent equipment, the adsorbent equipment are used to adsorb tail gas in production of polysilicon, adsorb tail in production of polysilicon Dichlorosilane, trichlorosilane in gas, hydrogen chloride, tail gas in the production of polysilicon after absorption is obtained, it is described by inhaling Tail gas includes nitrogen and hydrogen in attached production of polysilicon;The adsorbent equipment is additionally operable to be taken off adsorbed material It is attached, tail gas in the production of polysilicon of desorption out is obtained, tail gas includes dichloro-dihydro in the production of polysilicon of the desorption out Silicon, trichlorosilane and hydrogen chloride;
Elution device, it is connected with the adsorbent equipment, the elution device is used for using the silicon tetrachloride containing liquid Elution liquid condensing simultaneously elutes tail gas in the production of polysilicon of the desorption out, obtains scrubbed leacheate and scrubbed Production of polysilicon in tail gas, the scrubbed leacheate includes silicon tetrachloride, dichlorosilane, trichlorosilane and chlorination Hydrogen.
By handling in production of polysilicon after the system of tail gas, tail gas key component in the production of polysilicon after absorption For nitrogen and hydrogen, can be directly vented after the alkali lye elution in the alkali lye elution device of subsequent technique;After scrubbed Tail gas key component is nitrogen and hydrogen in production of polysilicon, and wherein chlorosilane accounting is 1~5wt%, by subsequent technique Can directly it be vented after the elution of alkali lye elution device alkali lye, after scrubbed leacheate enters the rectifier unit separation of subsequent technique Put into recycling.
Preferably, the adsorbent equipment include the first adsorbing mechanism, the second adsorbing mechanism, first adsorbing mechanism with Second adsorbing mechanism alternately carries out adsorption and desorption to tail gas in production of polysilicon, obtains the polycrystalline after absorption Tail gas in tail gas, the production of polysilicon of the desorption out in silicon production.
Preferably, first adsorbing mechanism is connected with second adsorbing mechanism, when first adsorbing mechanism pair When tail gas is adsorbed in production of polysilicon, it can be used all or part obtained after first adsorbing mechanism absorption more Tail gas is desorbed to second adsorbing mechanism in crystal silicon production;
When tail gas adsorbs during second adsorbing mechanism is to production of polysilicon, can be used by the described second absorption Tail gas is desorbed to first adsorbing mechanism in all or part of production of polysilicon obtained after mechanism absorption.
Preferably, the adsorbent equipment includes the first adsorbing mechanism, the second adsorbing mechanism,
First adsorbing mechanism includes being arranged at the first entrance of described first adsorbing mechanism one end and first outlet, set The other end of second outlet of the first adsorbing mechanism is placed in, the first outlet is connected with the elution device;
Second adsorbing mechanism includes being arranged at the second entrance of described second adsorbing mechanism one end and the 3rd outlet, set Other end of 4th outlet of second adsorbing mechanism is placed in, the 3rd outlet is connected with the elution device;
Wherein, the second outlet connects with the described 4th outlet,
When first adsorbing mechanism is used to adsorb dichlorosilane in production of polysilicon in tail gas, trichlorosilane, chlorine When changing hydrogen, tail gas enters first adsorbing mechanism by the first entrance in production of polysilicon, after absorption, obtained warp Tail gas is discharged by the second outlet in the production of polysilicon crossed after absorption, can be by polysilicon of all or part after absorption Tail gas is redirected back into second adsorbing mechanism by the described 4th outlet in production, the material that second adsorbing mechanism is adsorbed Reversely it is desorbed, tail gas is discharged by the described 3rd outlet in the production of polysilicon for being desorbed out, enters the elution device;
When second adsorbing mechanism is used to adsorb dichlorosilane in production of polysilicon in tail gas, trichlorosilane, chlorine When changing hydrogen, tail gas enters second adsorbing mechanism by the second entrance in production of polysilicon, after absorption, obtained warp Tail gas in the production of polysilicon after absorption is crossed to be discharged by the described 4th outlet, can be by polysilicon of all or part after absorption Tail gas is redirected back into first adsorbing mechanism by the second outlet in production, the material that first adsorbing mechanism is adsorbed Reversely it is desorbed, tail gas is discharged by the first outlet in the production of polysilicon for being desorbed out, enters the elution device.
Preferably, first adsorbing mechanism is 3~6 adsorption columns, and second adsorbing mechanism is 3~6 absorption Post.
Preferably, the system of tail gas also includes heat exchanger in described processing production of polysilicon, and the heat exchanger is used for The adsorbent equipment is exchanged heat.
Preferably, the heat exchanger is arranged in the adsorbent equipment, and the heat exchanger includes being used to be passed through thermal conducting agent And the heat exchanger tube to be exchanged heat with the adsorbent equipment, the heat exchanger also include being arranged on the heat exchanger tube changing for increase The fin of hot area.
Preferably, the system of tail gas also includes supercharging device, the supercharging device in described processing production of polysilicon It is connected with the adsorbent equipment, the supercharging device is used for being carried out into tail gas in the production of polysilicon before the adsorbent equipment Supercharging.
The method and system of tail gas in processing production of polysilicon in the present invention, by being carried out to tail gas in production of polysilicon Absorption, obtain tail gas in the production of polysilicon after absorption, the tail gas enter subsequent technique alkali lye elution after can be direct Emptying;Again by the way that the material of absorption is desorbed, the tail gas in the production of polysilicon of desorption out is obtained, the master in the tail gas It is dichlorosilane, trichlorosilane and hydrogen chloride to want component, and the content of fixed gas therein is very low, so that what desorption came out Tail gas in production of polysilicon is good using the effect of silicon tetrachloride condensation elution, the dichlorosilane of wherein most, trichlorine hydrogen Silicon and hydrogen chloride are leached, and can be reclaimed into follow-up rectification working process, obtained scrubbed production of polysilicon Middle tail gas can be directly vented after entering the alkali lye elution of subsequent technique, the chlorine silicon in scrubbed production of polysilicon in tail gas The content of alkane and hydrogen chloride is very low, so being dropped significantly in the alkali lye consumption amount carried out used in the alkali lye elution of subsequent technique It is low.
Effective recovery of chlorosilane in tail gas can not be realized for existing cryogenic condensation technology, while continues to reduce condensation Temperature increases the defects of cooling medium consumption and equipment investment problem.The method of tail gas in processing production of polysilicon in the present invention And system, when can may be implemented in the identical chlorosilane rate of recovery in this way, elution low temperature silicon tetrachloride cooling medium disappears Consumption declines 30~50%, continues technique after entering by tail gas in the scrubbed production of polysilicon that is obtained after elution device The processing of alkali lye elution device when so that alkali lye consumption amount declines 30~50%, can be achieved at production of polysilicon tail gas hazard-free Reason.
Therefore, the present invention in processing production of polysilicon in tail gas method and system, realize polysilicon production process Effective processing of middle tail gas, the decline of production of polysilicon cost is realized, the harmless discharge of system tail gas, realizes production of polysilicon Transformation of the enterprise to innoxious, environmentally friendly chemical enterprise.
Brief description of the drawings
Fig. 1 is the structural representation of the system of tail gas in the processing production of polysilicon in the embodiment of the present invention 2;
Fig. 2 is the structural representation of the adsorbent equipment and heat exchanger in the embodiment of the present invention 2.
In figure:1- tail gas buffers;2- supercharging devices;The adsorbing mechanisms of 3- first;31- first entrances;32- first outlets; 33- second outlets;The adsorbing mechanisms of 4- second;41- second entrances;42- the 3rd is exported;43- the 4th is exported;5- elution devices;51- Eluting column;511- eluting column top exits;512- eluting column outlet at bottoms;52- cooling bodies;53- reflux pumps;6- heat exchanger tubes; 7- fins;8- support members;The valves of 9- first;The valves of 10- second;The valves of 11- the 3rd;The valves of 12- the 4th;The valves of 13- the 6th; The valves of 14- the 5th;The heat exchanger tubes of 15- first;The valves of 16- the 7th;The valves of 17- the 8th;The valves of 18- the 9th;The valves of 19- the tenth;20- Second heat exchanger tube;The valves of 21- the 11st;The valves of 22- the 12nd;The valves of 23- the 13rd;The valves of 24- the 14th;25- absorption dresses Put.
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 system for handling tail gas in production of polysilicon, in production of polysilicon tail gas include nitrogen, Hydrogen, dichlorosilane, trichlorosilane and hydrogen chloride, system include:
Adsorbent equipment, the adsorbent equipment are used to adsorb tail gas in production of polysilicon, adsorb tail in production of polysilicon Dichlorosilane, trichlorosilane in gas, hydrogen chloride, tail gas in the production of polysilicon after absorption is obtained, after absorption Production of polysilicon in tail gas include nitrogen and hydrogen;Adsorbent equipment is additionally operable to adsorbed material being desorbed, and is taken off Tail gas in attached production of polysilicon out, in the production of polysilicon for being desorbed out tail gas include dichlorosilane, trichlorosilane and Hydrogen chloride;
Elution device, it is connected with adsorbent equipment, elution device is used for cold using the leacheate of the silicon tetrachloride containing liquid Tail gas in the production of polysilicon that coalescence elution is desorbed out, obtains scrubbed leacheate and scrubbed polysilicon Tail gas in production, scrubbed leacheate include silicon tetrachloride, dichlorosilane, trichlorosilane and hydrogen chloride.
The present embodiment provides tail in a kind of system processing production of polysilicon using tail gas in above-mentioned processing production of polysilicon The method of gas, tail gas includes nitrogen, hydrogen, dichlorosilane, trichlorosilane and hydrogen chloride in production of polysilicon, method include with Lower step:
1) tail gas in production of polysilicon is adsorbed, adsorbs dichlorosilane, trichlorine in production of polysilicon in tail gas Hydrogen silicon, hydrogen chloride, tail gas in the production of polysilicon after absorption is obtained, tail gas includes in the production of polysilicon after absorption Nitrogen and hydrogen;
2) adsorbed material is desorbed, obtains tail gas in the production of polysilicon of desorption out, be desorbed out is more Tail gas includes dichlorosilane, trichlorosilane and hydrogen chloride in crystal silicon production;
3) tail gas in the production of polysilicon for being desorbed out is eluted using the leacheate of the silicon tetrachloride containing liquid, obtained The tail gas into scrubbed leacheate and scrubbed production of polysilicon, scrubbed leacheate include silicon tetrachloride, Dichlorosilane, trichlorosilane and hydrogen chloride.
By handling in production of polysilicon after the method and system of tail gas, tail gas master in the production of polysilicon after absorption It is nitrogen and hydrogen to want component, can be directly vented after the alkali lye elution of subsequent technique;Production of polysilicon after scrubbed Middle tail gas key component is nitrogen and hydrogen, and wherein chlorosilane accounting is 1~5wt%, and dress is eluted by the alkali lye of subsequent technique Can directly it be vented after putting alkali lye elution, scrubbed leacheate puts into profit again after entering the rectifier unit separation of subsequent technique In.
The method and system of tail gas in processing production of polysilicon in the present embodiment, by entering to tail gas in production of polysilicon Row absorption, obtains tail gas in the production of polysilicon after absorption, and the tail gas can be direct after entering follow-up alkali lye treatment process Emptying;Again by the way that the material of absorption is desorbed, the tail gas in the production of polysilicon of desorption out is obtained, the master in the tail gas It is dichlorosilane, trichlorosilane and hydrogen chloride to want component, and the content of fixed gas therein is very low, so that what desorption came out Tail gas in production of polysilicon is good using the effect of silicon tetrachloride condensation elution, the dichlorosilane of wherein most, trichlorine hydrogen Silicon and hydrogen chloride are leached, and can be reclaimed into follow-up rectification working process, obtained scrubbed production of polysilicon Middle tail gas can be directly vented after entering follow-up alkali lye treatment process, the chlorosilane in scrubbed production of polysilicon in tail gas It is very low with the content of hydrogen chloride, so being substantially reduced in the alkali lye consumption amount carried out used in follow-up alkali lye treatment process.
Effective recovery of chlorosilane in tail gas can not be realized for existing cryogenic condensation technology, while continues to reduce condensation Temperature increases the defects of cooling medium consumption and equipment investment problem.The side of tail gas in processing production of polysilicon in the present embodiment When method and system can may be implemented in the identical chlorosilane rate of recovery in this way, elution low temperature silicon tetrachloride cooling medium Consumption declines 30~50%, continues work after entering by tail gas in the scrubbed production of polysilicon that is obtained after elution device During the alkali lye elution device processing of skill so that alkali lye consumption amount declines 30~50%, and production of polysilicon tail gas hazard-free can be achieved Processing.
Therefore, in the processing production of polysilicon in the present embodiment tail gas method and system, realize production of polysilicon mistake Effective processing of tail gas in journey, the decline of production of polysilicon cost is realized, the harmless discharge of system tail gas, realizes that polysilicon is given birth to Produce transformation of the enterprise to innoxious, environmentally friendly chemical enterprise.
Embodiment 2
As shown in figure 1, the present embodiment provides a kind of system for handling tail gas in production of polysilicon, tail gas in production of polysilicon Including nitrogen, hydrogen, dichlorosilane, trichlorosilane and hydrogen chloride, system includes:
Tail gas buffer 1, for storing tail gas in production of polysilicon;Existing production of polysilicon enterprise is by production system Tail gas containing a large amount of hydrogen and chlorosilane is reclaimed, and the tail gas of discharge mainly contains a large amount of nitrogen, a small amount of hydrogen, dichloro Dihydro silicon, trichlorosilane and hydrogen chloride, by process pipelines by the unified collection of this partial tail gas in tail gas buffer 1.
Supercharging device 2, the supercharging device 2 are connected with tail gas buffer 1, before supercharging device 2 is used for entering adsorbent equipment Production of polysilicon in tail gas be pressurized;Tail gas is delivered to adsorbent equipment after the supercharging of supercharging device 2.Specifically, this implementation Supercharging device 2 in example is booster pump.
Adsorbent equipment, adsorbent equipment are connected with supercharging device 2, and the adsorbent equipment is used to carry out tail gas in production of polysilicon Adsorb, dichlorosilane, trichlorosilane in absorption production of polysilicon in tail gas, hydrogen chloride, obtain the polycrystalline after absorption Tail gas in silicon production, tail gas includes nitrogen and hydrogen in the production of polysilicon after absorption;Adsorbent equipment is additionally operable to be inhaled Attached material is desorbed, and obtains tail gas in the production of polysilicon of desorption out, tail gas bag in the production of polysilicon for being desorbed out Include dichlorosilane, trichlorosilane and hydrogen chloride;The adsorbent equipment being desorbed is cooled down, completed for adsorbent equipment again It is raw.
It should be noted that the adsorbent equipment in the present embodiment includes the first adsorbing mechanism 3, the second adsorbing mechanism 4,
First adsorbing mechanism 3 includes being arranged at the first entrance 31 of the one end of the first adsorbing mechanism 3 and first outlet 32, set In 3 other end of second outlet 33 of the first adsorbing mechanism, first outlet 32 is connected with elution device 5;Specifically, in the present embodiment First entrance 31 and first outlet 32 be arranged at the bottom of the first adsorbing mechanism 3, second outlet 33 is arranged at the first adsorption machine The top of structure 3.
Second adsorbing mechanism 4 includes being arranged at the outlet of second entrance 41 and the 3rd 42 of the one end of the second adsorbing mechanism 4, set In 4 other end of 4th outlet 43 of the second adsorbing mechanism, the 3rd outlet 42 is connected with elution device 5;Specifically, the present embodiment In the bottoms that are arranged at the second adsorbing mechanism 4 of the outlet of second entrance 41 and the 3rd 42, the 4th outlet 43 is arranged at the first absorption The top of mechanism 3.
Wherein, second outlet 33 is connected with the 4th outlet 43,
When the first adsorbing mechanism 3 is used to adsorb dichlorosilane in production of polysilicon in tail gas, trichlorosilane, hydrogen chloride When, tail gas enters the first adsorbing mechanism 3 by first entrance 31 in production of polysilicon, after absorption, obtain after absorption Production of polysilicon in tail gas discharged by second outlet 33, can be by tail gas in production of polysilicon of all or part after absorption Second adsorbing mechanism 4 is redirected back into by the 4th outlet 43, the material that the second adsorbing mechanism 4 adsorbs reversely is desorbed, is desorbed Tail gas enters elution device 5 by the discharge of the 3rd outlet 42 in production of polysilicon out;Specifically, part in the present embodiment Tail gas is redirected back into the second adsorbing mechanism 4 by the 4th outlet 43 in production of polysilicon after absorption, and remaining is by absorption Tail gas directly excludes to carry out the alkali lye elution device progress alkali lye elution processing of subsequent technique in production of polysilicon afterwards, after elution The main component of obtained tail gas is hydrogen and nitrogen, is directly vented.
When the second adsorbing mechanism 4 is used to adsorb dichlorosilane in production of polysilicon in tail gas, trichlorosilane, hydrogen chloride When, tail gas enters the second adsorbing mechanism 4 by second entrance 41 in production of polysilicon, after absorption, obtain after absorption Production of polysilicon in tail gas by the 4th outlet 43 discharge, can be by tail gas in production of polysilicon of all or part after absorption First adsorbing mechanism 3 is redirected back into by second outlet 33, the material that the first adsorbing mechanism 3 adsorbs reversely is desorbed, is desorbed Tail gas is discharged by first outlet 32 in production of polysilicon out, enters elution device 5.Specifically, part in the present embodiment Tail gas is redirected back into the first adsorbing mechanism 3 by second outlet 33 in production of polysilicon after absorption, and remaining is by absorption Tail gas directly excludes to carry out the alkali lye elution device progress alkali lye elution processing of subsequent technique in production of polysilicon afterwards, after elution The main component of obtained tail gas is hydrogen and nitrogen, is directly vented.
Elution device 5, is connected with adsorbent equipment, and elution device 5 is used for the leacheate using the silicon tetrachloride containing liquid Tail gas in the production of polysilicon for being desorbed out is condensed and eluted, obtains scrubbed leacheate and scrubbed polycrystalline Tail gas in silicon production, scrubbed leacheate include silicon tetrachloride, dichlorosilane, trichlorosilane and hydrogen chloride.Specifically Elution device 5 in the present embodiment includes eluting column 51, cooling body 52, reflux pump 53, and eluting column 51 is connected with adsorbent equipment, Eluting column 51 is used to elute the tail gas that adsorbent equipment is desorbed out, and cooling body 52 is connected with eluting column 51, cooler Structure 52 is used to condense the leacheate in eluting column 51.Eluting column 51 includes being used to discharge scrubbed production of polysilicon The eluting column top exit 511 of middle tail gas and the eluting column outlet at bottom 512 for discharging leacheate, reflux pump 53 respectively with leaching Wash tower bottom outlet 512 to connect with the entrance of cooling body 52, reflux pump 53 is used for the leaching that will be flowed out from eluting column outlet at bottom 512 Washing lotion is pumped into cooling body 52, and leacheate is after the cooling of cooling body 52, then is back in eluting column 51.
By handling in production of polysilicon after the method for tail gas, tail gas key component in the production of polysilicon after absorption For nitrogen and hydrogen, tail gas key component is nitrogen and hydrogen in scrubbed production of polysilicon.
In chlorosilane, hydrogen chloride and chlorosilane in adsorbent equipment in the present embodiment in addition adsorbent absorption tail gas Part phosphorus, boron impurity, adsorbent are modified activated carbon.Chlorine-containing silane or do not contain in tail gas in production of polysilicon after absorption There is a small amount of chlorosilane, tail gas is directly entered the alkali lye elution device progress alkali of subsequent technique in the production of polysilicon after absorption Liquid elution is handled, and the main component of the tail gas obtained after elution is hydrogen and nitrogen, is directly vented.
Tail gas in a small amount of production of polysilicon after absorption can be used to carry out anti-the adsorbent equipment after absorption Blow, adsorbed material can be desorbed, obtain tail gas in the production of polysilicon of desorption out and contain a small amount of fixed gas The tail gas of (nitrogen and hydrogen) and a large amount of chlorosilanes, enters back into elution device 5 and is condensed and eluted recovery chlorosilane.Due to The constituent content of fixed gas in the tail gas being leached is relatively low, can almost ignore, so being passed into the cold of elution device 5 Solidifying elution efficiency is high, and the tail gas being almost largely leached is condensed and eluted, in obtained scrubbed production of polysilicon Chlorosilane content in tail gas is relatively low, it is scrubbed after production of polysilicon in tail gas be directly entered the alkali lye of subsequent technique Elution device carries out alkali lye elution processing, can effectively reduce alkali lye consumption and chlorosilane loss amount.
Preferably, the first adsorbing mechanism 3 is 3~6 adsorption columns, and the second adsorbing mechanism 4 is 3~6 adsorption columns, operation Period has and only an adsorption column is adsorbed, and other adsorption columns are regenerated or activate or stand by.First inhales A how many adsorption column are needed to be operated in the adsorbing mechanism 4 of random structure 3 and second, can be according to the regeneration or activation of adsorption column Cycle length carries out setting combination.Preferably, combinations thereof can ensure that whole system is continuously worked.Wherein, adsorb Need to be activated before adsorbent first time use in post, adsorbent in adsorption column is used before once arriving and reusing afterwards Process needs to be regenerated.
It should be noted that the system of tail gas also includes heat exchanger in processing production of polysilicon in the present embodiment, exchange heat Device is used to exchange heat to adsorbent equipment.Specifically, as shown in Fig. 2 heat exchanger is arranged in adsorbent equipment 25, heat exchanger includes For the heat exchanger tube 6 for being passed through thermal conducting agent and being exchanged heat with adsorbent equipment 25, heat exchanger also includes being arranged on heat exchanger tube 6 being used for Increase the fin 7 of heat exchange area.Fin 7 can be exchanged heat in adsorbent equipment 25 with the adsorbent in adsorbent equipment 25, be carried High heat exchange efficiency.Adsorbent equipment 25 in the present embodiment is adsorption column, and heat exchanger tube 6 is shaped as U-typed, U-typed heat exchanger tube 6 Bottom is set close to the bottom of adsorption column, the top of U-typed heat exchanger tube 6 in the top of adsorption column, the cylinder of an adsorption column 4-8 heat exchanger tube 6 is equipped with, to ensure stabilization of the heat exchanger tube 6 in adsorption column, 3-5 support member 8 is provided with each adsorption column Fixed heat exchanger tube 6.
Specifically, the thermal conducting agent in the present embodiment is water, tail gas adsorbs in adsorbent equipment 25 is to production of polysilicon When, 0~70 DEG C of water at low temperature is passed through in heat exchanger, the material of absorption is cooled, adsorbent equipment 25 is removed in time and adsorbed The heat discharged in journey, improve adsorption efficiency;When tail gas is desorbed during adsorbent equipment 25 is to production of polysilicon, heat exchanger 100~180 DEG C of high-temperature water is inside passed through, is advantageous to the progress of desorption, is advantageous to accelerate the regeneration or activation of adsorbent equipment 25.
Specifically, the first adsorbing mechanism 3 in the present embodiment is an adsorption column, the second adsorbing mechanism 4 is an absorption Post.
Specifically, it is provided with the first valve on pipeline between the first entrance 31 of the adsorbing mechanism 3 of supercharging device 2 and first 9, the 3rd valve 11, the first adsorption machine are provided with the pipeline between the first outlet 32 and elution device 5 of the first adsorbing mechanism 3 The second valve 10 is provided with pipeline between the second outlet 33 and discharge duct of structure 3.
It is provided with the 4th valve 12 on pipeline between the second entrance 41 of the adsorbing mechanism 4 of supercharging device 2 and second, second The 6th valve 13 is provided with pipeline between 3rd outlet 42 of adsorbing mechanism 4 and elution device 5, the second adsorbing mechanism 4 The 5th valve 14 is provided with pipeline between 4th outlet 43 and discharge duct, and between the second valve 10 and discharge duct Pipeline binding between pipeline and the 5th valve 14 and discharge duct simultaneously connects.
Heat exchanger includes being arranged at First Heat Exchanger in the first adsorbing mechanism 3, the be arranged in the second adsorbing mechanism 4 Two heat exchangers.
It is provided with First Heat Exchanger in first adsorbing mechanism 3, First Heat Exchanger includes the first heat exchanger tube 15 and is arranged at the The first fin (being not drawn on figure) on one heat exchanger tube 15, the first heat exchanger tube 15 include being used to be passed through hot water to the first heat exchanger tube 15 The first hot water tube inlet, for from the first heat exchanger tube 15 release hot water the first hot-water line outlet, in the first hot water tube inlet Place is provided with the 7th valve 16, the 9th valve 18 is provided with the first hot-water line exit, and First Heat Exchanger also includes being used to lead to Enter the first cold water tube inlet of cold water, exported for releasing the first cold water pipe of cold water, is provided with the first cold water pipe porch 8th valve 17, the first cold water pipe exit are provided with the tenth valve 19.
It is provided with the second heat exchanger in second adsorbing mechanism 4, the second heat exchanger includes the second heat exchanger tube 20 and is arranged at the The second fin (being not drawn on figure) on two heat exchanger tubes 20, the second heat exchanger tube 20 include being used to be passed through hot water to the second heat exchanger tube 20 The second hot water tube inlet, for from the second heat exchanger tube 20 release hot water the second hot-water line outlet, in the second hot water tube inlet Place is provided with the 11st valve 21, the 13rd valve 23 is provided with the second hot-water line exit, and the second heat exchanger also includes using In being passed through the second cold water tube inlet of cold water, being exported for releasing the second cold water pipe of cold water, set in the second cold water pipe porch The 12nd valve 22 is equipped with, the second cold water pipe exit is provided with the 14th valve 24.
When the first adsorbing mechanism 3 is in adsorbed state, the second adsorbing mechanism 4 is in detachment status.By in production of polysilicon Tail gas is passed into the first adsorbing mechanism 3 after carrying out booster compression by supercharging device 2, opens the first valve 9, closes the 4th valve Door 12, tail gas switches to the first adsorbing mechanism 3 from the second adsorbing mechanism 4, due to the first adsorbing mechanism 3 completed desorption, most Regenerative process is completed eventually, and the 3rd valve 11 is closed mode.After tail gas enters the first adsorbing mechanism 3 in production of polysilicon, the Two valves 10, the 5th valve 14, the 6th valve 13 are synchronous to be opened, and tail gas is through the second valve in the production of polysilicon after absorption 10, which flow to discharge duct, leaves the first adsorbing mechanism 3, and the alkali lye elution device for being partly into subsequent technique carries out alkali lye elution Processing, another part after the 5th valve 14 by being reversely blown into the second adsorbing mechanism 4.The of synchronous second hot-water line porch 11 valves 21, the 13rd valve 23 in the second hot-water line exit are opened, and are desorbed to the second adsorbing mechanism 4 and are provided heat, the The material of two adsorbing mechanisms 4 absorption is in the production of polysilicon after absorption from the second adsorption machine in the presence of tail gas and heat It is desorbed on structure 4, the tail gas containing a large amount of chlorosilanes enters elution device 5 through the 6th valve 13 after desorption, in elution device 5 The elution liquid condensing of silicon tetrachloride of the interior use containing liquid simultaneously elutes the tail gas of desorption out, and the elution for carrying out chlorosilane is returned Receive.After the second adsorbing mechanism 4 is desorbed certain time, the 6th valve 13 and the 5th valve 14 are closed, stopping will pass through first and inhale Tail gas is passed into the second adsorbing mechanism 4 in production of polysilicon after the absorption of random structure 3, while will synchronous second hot water tube inlet 11st valve 21, the 13rd valve 23 in the second hot-water line exit at place are closed.The second cold water pipe porch is opened again to set The 12nd valve 22, the 14th valve 24 of the second cold water pipe exit setting put, cool to the second adsorbing mechanism 4, After the temperature of the second adsorbing mechanism 4 drops to a certain degree, the second adsorbing mechanism 4 reaches stand-by state, and the first adsorbing mechanism 3 enters Detachment status.
When the second adsorbing mechanism 4 is in adsorbed state, the first adsorbing mechanism 3 is in detachment status.By in production of polysilicon Tail gas is passed into the second adsorbing mechanism 4 after carrying out booster compression by supercharging device 2, opens the 4th valve 12, closes first Valve 9, tail gas switch to the second adsorbing mechanism 4 from the first adsorbing mechanism 3, due to the second adsorbing mechanism 4 completed desorption, most Regenerative process is completed eventually, and the 6th valve 13 is closed mode.After tail gas enters the second adsorbing mechanism 4 in production of polysilicon, the Five valves 14, the second valve 10, the 3rd valve 11 are synchronous to be opened, and tail gas is through the 5th valve in the production of polysilicon after absorption 14, which flow to discharge duct, leaves the second adsorbing mechanism 4, and the alkali lye elution device for being partly into subsequent technique enters at alkali lye elution Reason, another part after the second valve 10 by being reversely blown into the first adsorbing mechanism 3.The 7th of synchronous first hot-water line porch Valve 16, the 9th valve 18 in the first hot-water line exit are opened, and are desorbed to the first adsorbing mechanism 3 and are provided heat, the first absorption The material that mechanism 3 is adsorbed is in the production of polysilicon after absorption in the presence of tail gas and heat from the first adsorbing mechanism 3 Desorption gets off, and the tail gas containing a large amount of chlorosilanes enters elution device 5 through the 3rd valve 11 after desorption, makes in elution device 5 With the elution liquid condensing of the silicon tetrachloride containing liquid and the tail gas of desorption out is eluted, carries out the elution recovery of chlorosilane. After first adsorbing mechanism 3 desorption certain time, the second adsorbing mechanism will be passed through by closing the 3rd valve 11 and the second valve 10, stopping Tail gas is passed into the first adsorbing mechanism 3 in production of polysilicon after 4 absorption, while by the of synchronous first hot-water line porch Seven valves 16, the 9th valve 18 in the first hot-water line exit are closed.The 8th valve of the first cold water pipe porch setting is opened again The tenth valve 19 that the 17, second cold water pipe exit of door is set, cools to the first adsorbing mechanism 3, when the first adsorbing mechanism 3 After temperature drops to a certain degree, the first adsorbing mechanism 3 reaches stand-by state, and the second adsorbing mechanism 4 enters detachment status.
Said process circulation is carried out.It is achieved thereby that the processing of the serialization of whole system, substantially increases operating efficiency.
The elution liquid condensing of the silicon tetrachloride containing liquid in scrubbed device 5 simultaneously elutes the polysilicon of desorption out Tail gas directly outer can be discharged in air in production.
Tail gas mainly contains nitrogen and hydrogen in production of polysilicon after absorption, enters subsequent technique using pressure difference Alkali lye elution device carries out alkali lye elution processing, and the tail gas after processing can directly carry out arranging outside, the polysilicon life after absorption Tail gas is used to be desorbed the adsorbent equipment after other absorption in production.
Tail gas fills after the modified activated carbon Adsorption Concentration in adsorbent equipment using by other absorption in production of polysilicon Tail gas in the production of polysilicon after absorption is put, the heat exchanger tube 6 with fin 7 is carried out under conditions of being passed through hot water in adsorbent equipment The desorption of chlorosilane, the chlorosilane gas containing a small amount of fixed gas after desorption are eluted into elution device 5, for chlorine silicon The recovery of alkane, it is -40~0 DEG C that elution, which uses the temperature of silicon tetrachloride, the chlorine in scrubbed rear production of polysilicon in tail gas Silane accounting is 1~5%, and the alkali lye elution device of tail gas into subsequent technique enters in production of polysilicon after this part is scrubbed Outer arrange is carried out after row alkali lye elution processing.Due to after adsorption/desorption so that in the production of polysilicon for being desorbed out in tail gas The content of fixed gas substantially reduce, can so greatly improve condensation point so that tail gas in the production of polysilicon for being desorbed out It is easier to make for condensing.The method of the present embodiment can be carried out elution and absorb be desorbed out under relatively high condensation temperature Chlorosilane and hydrogen chloride in production of polysilicon in tail gas.
Preferably, adsorbent equipment includes the first adsorbing mechanism 3, the second adsorbing mechanism 4, the first adsorbing mechanism 3 and second Adsorbing mechanism 4 alternately carries out adsorption and desorption to tail gas in production of polysilicon, obtains tail in the production of polysilicon after absorption Tail gas in gas, the production of polysilicon of desorption out.Certainly, the first adsorbing mechanism 3 can also be not connected to the second adsorbing mechanism 4, As long as meeting both, alternately adsorption and desorption works.
It is further preferred that the first adsorbing mechanism 3 is connected with the second adsorbing mechanism 4, when the first adsorbing mechanism 3 is given birth to polysilicon When tail gas is adsorbed in production, it can be used in all or part of production of polysilicon obtained after the absorption of the first adsorbing mechanism 3 Tail gas is desorbed to the second adsorbing mechanism 4;It can so avoid introducing what foreign gas was desorbed the first adsorbing mechanism 3 Step, and can cause after the first adsorbing mechanism 3 adsorbs in obtained all or part of production of polysilicon tail gas continue into Enter the second adsorbing mechanism 4 to carry out after after-treatment being handled in follow-up technique again.
When tail gas adsorbs during the second adsorbing mechanism 4 is to production of polysilicon, it can be used and inhaled by the second adsorbing mechanism 4 Tail gas is desorbed to the first adsorbing mechanism 3 in attached obtained all or part of production of polysilicon.It can so avoid introducing The step of foreign gas is desorbed to the second adsorbing mechanism 4, and can cause what is obtained after the second adsorbing mechanism 4 adsorbs Tail gas goes successively to the first adsorbing mechanism 3 and carries out after after-treatment entering in follow-up technique again in all or part of production of polysilicon Row processing.
The present embodiment provides tail in a kind of system processing production of polysilicon using tail gas in above-mentioned processing production of polysilicon The method of gas, tail gas includes nitrogen, hydrogen, dichlorosilane, trichlorosilane and hydrogen chloride in production of polysilicon, method include with Lower step:
1) tail gas in the production of polysilicon before adsorbing is carried out being pressurized to 0.5Mpa.
2) tail gas in production of polysilicon is adsorbed at 30 DEG C, adsorbs the dichloro-dihydro in tail gas in production of polysilicon Silicon, trichlorosilane, hydrogen chloride, tail gas in the production of polysilicon after absorption is obtained, in the production of polysilicon after absorption Tail gas includes nitrogen and hydrogen;And tail gas key component is nitrogen and hydrogen in the production of polysilicon after absorption.Preferably It is that the adsorption step can also adsorb in production of polysilicon the impurity containing boron, phosphorus in tail gas.Specifically, in the present embodiment Adsorbent used in adsorption step is modified activated carbon, dichlorosilane in adsorbable production of polysilicon in tail gas, Trichlorosilane, hydrogen chloride and the impurity containing boron, phosphorus.
3) adsorbed material is desorbed using tail gas in the obtained production of polysilicon after absorption, desorption Temperature is 100 DEG C, obtains tail gas in the production of polysilicon of desorption out, and tail gas includes dichloro in the production of polysilicon for being desorbed out Dihydro silicon, trichlorosilane and hydrogen chloride.
4) using the leacheate of the silicon tetrachloride containing liquid in the production of polysilicon that -20 DEG C of elution have been desorbed out Tail gas, obtains tail gas in scrubbed leacheate and scrubbed production of polysilicon, and scrubbed leacheate includes four Silicon chloride, dichlorosilane, trichlorosilane and hydrogen chloride.And tail gas key component is nitrogen in scrubbed production of polysilicon And hydrogen.Impurity concentration containing boron, phosphorus in scrubbed leacheate has reached relatively low level, through follow-up rectifying The production of polysilicon is can be directly used for after the separation of tower component.Due to after adsorption/desorption so that the polysilicon life for being desorbed out The content of fixed gas in production in tail gas substantially reduces, and can so greatly improve condensation point so that the polysilicon for being desorbed out Tail gas is easier to make for condensing in production.The method of the present embodiment can carry out elution absorption under relatively high condensation temperature Chlorosilane and hydrogen chloride in the production of polysilicon of desorption out in tail gas, realize effective recovery to chlorosilane in tail gas, Reduce cooling medium consumption and equipment investment.
By handling in production of polysilicon after the method and system of tail gas, tail gas master in the production of polysilicon after absorption It is nitrogen and hydrogen to want component, can be directly vented after the alkali lye elution of subsequent technique;Production of polysilicon after scrubbed Middle tail gas key component is nitrogen and hydrogen, and wherein chlorosilane accounting is 1~5wt%, and dress is eluted by the alkali lye of subsequent technique Can directly it be vented after putting alkali lye elution, scrubbed leacheate puts into profit again after entering the rectifier unit separation of subsequent technique In.
The method and system of tail gas in processing production of polysilicon in the present embodiment, by entering to tail gas in production of polysilicon Row absorption, obtains tail gas in the production of polysilicon after absorption, and the tail gas can be direct after entering follow-up alkali lye treatment process Emptying;Again by the way that the material of absorption is desorbed, the tail gas in the production of polysilicon of desorption out is obtained, the master in the tail gas It is dichlorosilane, trichlorosilane and hydrogen chloride to want component, and the content of fixed gas therein is very low, so that what desorption came out Tail gas in production of polysilicon is good using the effect of silicon tetrachloride condensation elution, the dichlorosilane of wherein most, trichlorine hydrogen Silicon and hydrogen chloride are leached, and can be reclaimed into follow-up rectification working process, obtained scrubbed production of polysilicon Middle tail gas can be directly vented after entering follow-up alkali lye treatment process, the chlorosilane in scrubbed production of polysilicon in tail gas It is very low with the content of hydrogen chloride, so being substantially reduced in the alkali lye consumption amount carried out used in follow-up alkali lye treatment process.
Effective recovery of chlorosilane in tail gas can not be realized for existing cryogenic condensation technology, while continues to reduce condensation Temperature increases the defects of cooling medium consumption and equipment investment problem.The side of tail gas in processing production of polysilicon in the present embodiment When method and system can may be implemented in the identical chlorosilane rate of recovery in this way, elution low temperature silicon tetrachloride cooling medium Consumption declines 30~50%, is continued after entering by tail gas in the scrubbed production of polysilicon that is obtained after elution device 5 During the alkali lye elution device processing of technique so that alkali lye consumption amount declines 30~50%, and it is harmless that production of polysilicon tail gas can be achieved Change is handled.
Therefore, in the processing production of polysilicon in the present embodiment tail gas method and system, realize production of polysilicon mistake Effective processing of tail gas in journey, the decline of production of polysilicon cost is realized, the harmless discharge of system tail gas, realizes that polysilicon is given birth to Produce transformation of the enterprise to innoxious, environmentally friendly chemical enterprise.
Preferably, the system also includes alkali lye elution device, and alkali lye elution device is connected with elution device, alkali lye elution Device is used to tail gas in the production of polysilicon after absorption carrying out alkali lye elution, the tail gas after emptying elution.Or alkali lye Elution device is also connected with adsorbent equipment, and tail gas carries out alkali lye elution in scrubbed production of polysilicon, after emptying elution Tail gas.
Preferably, the system also includes rectifier unit, and rectifier unit is connected with elution device, and rectifier unit is used for will be through The leacheate for crossing elution separates dichlorosilane and trichlorosilane by rectifying.
Embodiment 3
The present embodiment provides a kind of system processing polysilicon life of tail gas in processing production of polysilicon using in embodiment 2 The method of tail gas in production, tail gas includes nitrogen, hydrogen, dichlorosilane, trichlorosilane and hydrogen chloride, method in production of polysilicon Comprise the following steps:
1) tail gas in the production of polysilicon before adsorbing is carried out being pressurized to 0.1Mpa.
2) tail gas in production of polysilicon is adsorbed at 0 DEG C, adsorb dichlorosilane in production of polysilicon in tail gas, Trichlorosilane, hydrogen chloride, tail gas in the production of polysilicon after absorption is obtained, tail gas in the production of polysilicon after absorption Including nitrogen and hydrogen;And tail gas key component is nitrogen and hydrogen in the production of polysilicon after absorption.Preferably, should Adsorption step can also adsorb in production of polysilicon the impurity containing boron, phosphorus in tail gas.Specifically, the absorption step in the present embodiment Adsorbent used in rapid is modified activated carbon, dichlorosilane, trichlorine hydrogen in adsorbable production of polysilicon in tail gas Silicon, hydrogen chloride and the impurity containing boron, phosphorus.
3) adsorbed material is desorbed using tail gas in the obtained production of polysilicon after absorption, desorption Temperature is 180 DEG C, obtains tail gas in the production of polysilicon of desorption out, and tail gas includes dichloro in the production of polysilicon for being desorbed out Dihydro silicon, trichlorosilane and hydrogen chloride.
4) leacheate of silicon tetrachloride of the use containing liquid tail in the production of polysilicon that 0 DEG C of elution has been desorbed out Gas, obtains tail gas in scrubbed leacheate and scrubbed production of polysilicon, and scrubbed leacheate includes tetrachloro SiClx, dichlorosilane, trichlorosilane and hydrogen chloride.And in scrubbed production of polysilicon tail gas key component be nitrogen and Hydrogen.Impurity concentration containing boron, phosphorus in scrubbed leacheate has reached relatively low level, through follow-up rectifying column The production of polysilicon is can be directly used for after component separation.
The method of tail gas can may be implemented in identical chlorine in this way in processing production of polysilicon in the present embodiment During the silane rate of recovery, elution declines 30~50% with low temperature silicon tetrachloride cooling dielectric dissipation amount, passes through the warp obtained after elution Cross elution production of polysilicon in tail gas after entering continue technique alkali lye elution device processing when so that alkali lye consumption amount decline 30~50%, the processing of production of polysilicon tail gas hazard-free can be achieved.
Embodiment 4
The present embodiment provides a kind of system processing polysilicon life of tail gas in processing production of polysilicon using in embodiment 2 The method of tail gas in production, tail gas includes nitrogen, hydrogen, dichlorosilane, trichlorosilane and hydrogen chloride, method in production of polysilicon Comprise the following steps:
1) tail gas in the production of polysilicon before adsorbing is carried out being pressurized to 0.2Mpa.
2) tail gas in production of polysilicon is adsorbed at 70 DEG C, adsorbs the dichloro-dihydro in tail gas in production of polysilicon Silicon, trichlorosilane, hydrogen chloride, tail gas in the production of polysilicon after absorption is obtained, in the production of polysilicon after absorption Tail gas includes nitrogen and hydrogen;And tail gas key component is nitrogen and hydrogen in the production of polysilicon after absorption.Preferably It is that the adsorption step can also adsorb in production of polysilicon the impurity containing boron, phosphorus in tail gas.Specifically, in the present embodiment Adsorbent used in adsorption step is modified activated carbon, dichlorosilane in adsorbable production of polysilicon in tail gas, Trichlorosilane, hydrogen chloride and the impurity containing boron, phosphorus.
3) adsorbed material is desorbed using tail gas in the obtained production of polysilicon after absorption, desorption Temperature is 140 DEG C, obtains tail gas in the production of polysilicon of desorption out, and tail gas includes dichloro in the production of polysilicon for being desorbed out Dihydro silicon, trichlorosilane and hydrogen chloride.
4) using the leacheate of the silicon tetrachloride containing liquid in the production of polysilicon that -40 DEG C of elution have been desorbed out Tail gas, obtains tail gas in scrubbed leacheate and scrubbed production of polysilicon, and scrubbed leacheate includes four Silicon chloride, dichlorosilane, trichlorosilane and hydrogen chloride.And tail gas key component is nitrogen in scrubbed production of polysilicon And hydrogen.Impurity concentration containing boron, phosphorus in scrubbed leacheate has reached relatively low level, through follow-up rectifying The production of polysilicon is can be directly used for after the separation of tower component.
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 (14)

1. a kind of method for handling tail gas in production of polysilicon, tail gas includes nitrogen, hydrogen, dichloro two in the production of polysilicon Hydrogen silicon, trichlorosilane and hydrogen chloride, it is characterised in that the described method comprises the following steps:
Tail gas in production of polysilicon is adsorbed, dichlorosilane, trichlorosilane in absorption production of polysilicon in tail gas, chlorine Change hydrogen, obtain tail gas in the production of polysilicon after absorption;
Adsorbed material is desorbed, obtains tail gas in the production of polysilicon of desorption out;
Using the silicon tetrachloride containing liquid elution liquid condensing and elute it is described desorption out production of polysilicon in tail gas, obtain The tail gas into scrubbed leacheate and scrubbed production of polysilicon.
2. the method for tail gas in processing production of polysilicon according to claim 1, it is characterised in that the adsorption step is also The impurity containing boron, phosphorus in tail gas can be adsorbed in production of polysilicon.
3. the method for tail gas in processing production of polysilicon according to claim 1 or 2, it is characterised in that the absorption step Suddenly adsorbed using adsorbent, the adsorbent is modified activated carbon.
4. the method for tail gas in processing production of polysilicon according to claim 1, it is characterised in that the adsorption step Temperature is 0~70 DEG C, and the temperature of the desorption is 100~180 DEG C, and the temperature of the rinsing step is -40~0 DEG C.
5. the method for tail gas in processing production of polysilicon according to claim 1, it is characterised in that it is described will be adsorbed The step of material is desorbed be specially:Using tail gas in the obtained production of polysilicon after absorption to adsorbed material It is desorbed.
6. the method for tail gas in processing production of polysilicon according to claim 1, it is characterised in that also including following step Suddenly:
Tail gas in production of polysilicon before adsorbing is carried out being pressurized to 0.1~0.5Mpa.
7. a kind of system for handling tail gas in production of polysilicon, tail gas includes nitrogen, hydrogen, dichloro two in the production of polysilicon Hydrogen silicon, trichlorosilane and hydrogen chloride, it is characterised in that the system includes:
Adsorbent equipment, the adsorbent equipment are used to adsorb tail gas in production of polysilicon, adsorb in production of polysilicon in tail gas Dichlorosilane, trichlorosilane, hydrogen chloride, obtain tail gas in the production of polysilicon after absorption;The adsorbent equipment is also For adsorbed material to be desorbed, tail gas in the production of polysilicon of desorption out is obtained;
Elution device, it is connected with the adsorbent equipment, the elution device is used for the elution using the silicon tetrachloride containing liquid Liquid condensing simultaneously elutes tail gas in the production of polysilicon of the desorption out, obtains scrubbed leacheate and scrubbed more Tail gas in crystal silicon production.
8. the system of tail gas in processing production of polysilicon according to claim 7, it is characterised in that the adsorbent equipment bag The first adsorbing mechanism, the second adsorbing mechanism are included, first adsorbing mechanism replaces with second adsorbing mechanism gives birth to polysilicon Tail gas carries out adsorption and desorption in production, obtains tail gas in the production of polysilicon after absorption, the polycrystalline of the desorption out Tail gas in silicon production.
9. the system of tail gas in processing production of polysilicon according to claim 8, it is characterised in that first adsorption machine Structure is connected with second adsorbing mechanism, when tail gas adsorbs during first adsorbing mechanism is to production of polysilicon, can be made With tail gas in all or part of production of polysilicon obtained after first adsorbing mechanism absorption to second adsorption machine Structure is desorbed;
When tail gas adsorbs during second adsorbing mechanism is to production of polysilicon, it can be used and pass through second adsorbing mechanism Tail gas is desorbed to first adsorbing mechanism in all or part of production of polysilicon obtained after absorption.
10. the system of tail gas in processing production of polysilicon according to claim 7, it is characterised in that the adsorbent equipment Including the first adsorbing mechanism, the second adsorbing mechanism,
First adsorbing mechanism includes being arranged at the first entrance of described first adsorbing mechanism one end and first outlet, is arranged at The other end of second outlet of first adsorbing mechanism, the first outlet are connected with the elution device;
Second adsorbing mechanism includes being arranged at the second entrance of described second adsorbing mechanism one end and the 3rd outlet, is arranged at Other end of 4th outlet of second adsorbing mechanism, the 3rd outlet is connected with the elution device;
Wherein, the second outlet connects with the described 4th outlet,
When first adsorbing mechanism is used to adsorb dichlorosilane in production of polysilicon in tail gas, trichlorosilane, hydrogen chloride When, tail gas enters first adsorbing mechanism by the first entrance in production of polysilicon, after absorption, obtain by inhaling Tail gas is discharged by the second outlet in attached production of polysilicon, can be by production of polysilicon of all or part after absorption Middle tail gas is redirected back into second adsorbing mechanism by the described 4th outlet, and the material of second adsorbing mechanism absorption is carried out Reversely it is desorbed, tail gas is discharged by the described 3rd outlet in the production of polysilicon for being desorbed out, enters the elution device;
When second adsorbing mechanism is used to adsorb dichlorosilane in production of polysilicon in tail gas, trichlorosilane, hydrogen chloride When, tail gas enters second adsorbing mechanism by the second entrance in production of polysilicon, after absorption, obtain by inhaling Tail gas is discharged by the described 4th outlet in attached production of polysilicon, can be by production of polysilicon of all or part after absorption Middle tail gas is redirected back into first adsorbing mechanism by the second outlet, and the material of first adsorbing mechanism absorption is carried out Reversely it is desorbed, tail gas is discharged by the first outlet in the production of polysilicon for being desorbed out, enters the elution device.
11. the system of tail gas in processing production of polysilicon according to claim 10, it is characterised in that first absorption Mechanism is 3~6 adsorption columns, and second adsorbing mechanism is 3~6 adsorption columns.
12. the system of tail gas in processing production of polysilicon according to claim 7, it is characterised in that also including heat exchanger, The heat exchanger is used to exchange heat to the adsorbent equipment.
13. the system of tail gas in processing production of polysilicon according to claim 12, it is characterised in that the heat exchanger is set It is placed in the adsorbent equipment, the heat exchanger includes being used to be passed through thermal conducting agent and the heat exchange to be exchanged heat with the adsorbent equipment Pipe, the heat exchanger, which also includes being arranged at, is used for the fin for increasing heat exchange area on the heat exchanger tube.
14. the system of tail gas in processing production of polysilicon according to claim 7, it is characterised in that also include supercharging dress Put, the supercharging device is connected with the adsorbent equipment, and the supercharging device is used for the polycrystalline before the entrance adsorbent equipment Tail gas is pressurized in silicon production.
CN201610592188.2A 2016-07-26 2016-07-26 The method and system of tail gas in a kind of processing production of polysilicon Pending CN107648979A (en)

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