CN108726481A - A kind of processing unit of polycrystalline silicon reduction exhaust - Google Patents

A kind of processing unit of polycrystalline silicon reduction exhaust Download PDF

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Publication number
CN108726481A
CN108726481A CN201710240227.7A CN201710240227A CN108726481A CN 108726481 A CN108726481 A CN 108726481A CN 201710240227 A CN201710240227 A CN 201710240227A CN 108726481 A CN108726481 A CN 108726481A
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chlorosilane
liquid
scrubbing tower
hydrogen
gas
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CN108726481B (en
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陈世涛
王文
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Xinjiang Xinte Crystal Silicon High Tech Co.,Ltd.
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Xinte Energy Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D50/00—Combinations of methods or devices for separating particles from gases or vapours
    • B01D50/60—Combinations of devices covered by groups B01D46/00 and B01D47/00
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation 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
    • B01D53/002—Separation 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 condensation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation 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
    • B01D53/02—Separation 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/02—Silicon
    • C01B33/021—Preparation
    • C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
    • C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/16—Hydrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/20—Halogens or halogen compounds
    • B01D2257/204—Inorganic halogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0415—Purification by absorption in liquids
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/042—Purification by adsorption on solids

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Combustion & Propulsion (AREA)
  • Treating Waste Gases (AREA)
  • Silicon Compounds (AREA)

Abstract

The present invention provides a kind of processing unit of polycrystalline silicon reduction exhaust, including：Scrubbing tower for carrying out elution processing to reduction tail gas, and exports silicon powder-containing chlorosilane liquid produced from tower reactor, fixed gas is exported from tower top；Circulating pump protection location, for exporting chlorosilane liquid produced after removing silica flour and impurity in silicon powder-containing chlorosilane liquid produced；Scrubbing tower circulating pump participates in elution work for being sent back to after being pressurized chlorosilane liquid produced inside scrubbing tower；Dust removing units obtain the fixed gas after dedusting for removing the silica flour in fixed gas；Chlorosilane therein is all condensed out and is sent to chlorosilane condensate liquid collecting tank, while exporting and containing impurity hydrogen by multistage cooling unit for making the fixed gas after dedusting pass through multistage cooling treatment successively；Multistage activated carbon adsorption unit obtains pure hydrogen and is sent to hydrogen gas buffer for making the multi-stage absorption of passing through successively containing impurity hydrogen of multistage cooling unit output handle.The present invention can effectively remove the silica flour in reduction tail gas.

Description

A kind of processing unit of polycrystalline silicon reduction exhaust
Technical field
The present invention relates to technical field of polysilicon production, and in particular to a kind of processing unit of polycrystalline silicon reduction exhaust.
Background technology
Polysilicon is key raw material used by integrated circuit and photovoltaic generation, is necessary to national new energy development Raw material.In the epoch of the worsening shortages of fossil energy instantly, the emergence of novel energy has become inexorable trend.
In the polysilicon production process in China, 90% production of polysilicon enterprise all uses improved Siemens polysilicon Production technology carries out the production of polysilicon, while reduction apparatus is generated using CDI devices (i.e. tail gas dry process retracting device) Tail gas (restoring tail gas) is recycled.Specifically, to hydrogen and chlorosilane progress separating treatment in reduction tail gas, so The impurity contained in the hydrogen that CDI devices are separated is removed afterwards, and it is made to repeat to enter in reduction apparatus, is made for producing With；The chlorosilane that CDI devices are separated is transported to rectifier unit, silicon tetrachloride is separated, and is delivered to cold hydrogen It is used as raw material in change or hot hydrogenation apparatus, produces trichlorosilane again, is then fed into reduction apparatus and participates in reduction reaction, and The trichlorosilane and dichlorosilane separated from rectifier unit, which are then sent directly into reduction apparatus, participates in reduction reaction, with life Produce polysilicon.
In improved Siemens polysilicon production process, the characteristics of vent gas treatment flow of CDI devices is to make to go back protocercal tail Gas passes through water recirculator, brine cooler, freon cooler and is cooled down successively, thus by most of chlorosilane condensate Get off, hydrogen is made to be detached with chlorosilane, the hydrogen separated carries out compression processing through hydrogen compressor, and compressed hydrogen enters suction Receive tower washing, through -44 DEG C cycle chlorosilanes washing after be re-fed into active carbon adsorption column, with absorb be mingled in hydrogen it is a small amount of Chlorosilane, HCl, PH3Deng, be then fed into reduction apparatus, repeat participate in production.The cycle chlorine silicon after hydrogen is washed in absorption tower Alkane is sent into Analytic Tower, will wherein HCl, dichlorosilane, PH3Part chlorosilane after evaporation by pump pressurize be sent into absorption tower with It recycles, while flap portion chlorosilane is delivered to rectification working process.
Inventor has found, is handled that there is three big defects to reduction tail gas using CDI devices：
First, the silica flour of CDI devices is brought into after can not effectively removing also original production by tail gas.The silica flour brought into will make Tower, the pump of CDI devices are blocked, are worn, and so as to cause equipment damage or system shutdown, and can be impacted to downstream process.
Second is that CDI plant energy consumptions are higher.By being found after carrying out data statistics to some domestic production of polysilicon enterprises, In the production of polysilicon enterprise of 10,000 tons, production 8.2 ten thousand KWhs/ton of silicon of total power consumption average out to of polysilicon, and CDI device power consumptions are flat The 15% of the total power consumption of production of polysilicon is accounted for, 1.2 ten thousand KWhs/ton of silicon are reached.
Third, system is huge, equipment is huge more, overhauls, is difficult in maintenance.The CDI devices of the polysilicon enterprise of 10,000 tons take up an area Area reaches 12000m2More than, investment reaches 200,000,000 yuan or more, all kinds of towers, pump, heat exchanger, compressor, refrigerator, slot, tank etc. Equipment reaches as many as 200, and each covering device damages, and polycrystalline silicon production line part or total system may all be caused to stop.
The above reason leads to cost increase in polysilicon production process, and the system failure is frequent, and enterprise competitiveness is caused to decline.
Invention content
The technical problem to be solved by the present invention is to for the drawbacks described above in the presence of the prior art, provide a kind of polycrystalline The processing unit of Si reduction tail gas can effectively remove the silica flour in reduction tail gas, the processing energy of reduction tail gas is greatly lowered Consumption, substantially reduction restore equipment amount needed for vent gas treatment.
Technical solution is used by solving present invention problem：
The present invention provides a kind of processing unit of polycrystalline silicon reduction exhaust, the reduction tail gas include hydrogen, chlorosilane and The gaseous mixture of a small amount of silica flour, the processing unit include：
Scrubbing tower, for carrying out elution processing to the reduction tail gas using top-down chlorosilane leacheate in tower, And silicon powder-containing chlorosilane liquid produced is exported from tower reactor, fixed gas is exported from tower top, the fixed gas includes hydrogen, unabsorbed chlorine The gaseous mixture of silane and silica flour；
Circulating pump protection location, the silica flour and impurity in silicon powder-containing chlorosilane liquid produced for removing the output of scrubbing tower tower reactor After export chlorosilane liquid produced；
Scrubbing tower circulating pump, through scrubbing tower top after the chlorosilane liquid produced supercharging for exporting circulating pump protection location Level-one spray port, which is sent into inside scrubbing tower, participates in elution work；
Dust removing units, the silica flour in fixed gas for removing washing column overhead output, obtain the fixed gas after dedusting；
Multistage cooling unit, for making the fixed gas after dedusting pass through multistage cooling treatment successively, by not coagulating after dedusting Chlorosilane in gas all condenses out and is sent to chlorosilane condensate liquid collecting tank, while exporting and containing impurity hydrogen；
Multistage activated carbon adsorption unit, for making being inhaled successively by multistage containing impurity hydrogen for multistage cooling unit output Attached processing obtains pure hydrogen and is sent to hydrogen gas buffer.
Optionally, the circulating pump protection location includes the first differential pressure indicator, the first control unit and two ceramic filters, Two ceramic filters are connected in parallel, and one opens one standby, and first differential pressure indicator enters with two ceramic filters respectively Mouth and outlet connection, the front and back pressure difference for measuring ceramic filter in operating status, first control unit are used for Ceramic filter in operating status is cut off when the measured value of the first differential pressure indicator is more than 0.1MPa, while will be in spare The ceramic filter of state is switched to operating status.
Optionally, the circulating pump protection location further includes liquid-level switch tank, is gone out respectively with two ceramic filters Mouth is connected with the entrance of scrubbing tower circulating pump, liquid-level switch is provided on liquid-level switch tank, for measuring in liquid-level switch tank Liquid level, first control unit stop the interlocking of scrubbing tower circulating pump when being additionally operable to the liquid level in liquid-level switch tank less than 70% Vehicle.
Optionally, it is additionally provided with pressure gauge on the liquid-level switch tank, for measuring the fluid pressure in liquid-level switch tank, First control unit interlocks scrubbing tower circulating pump when being additionally operable to the fluid pressure in liquid-level switch tank less than 0.1MPa Parking.
Optionally, the bottom of the scrubbing tower is provided with vertical isolating strainer, is used for the bottom section in scrubbing tower Be separated into spray liquid zone and pumping liquid zone, and scrubbing tower circulating pump through circulating pump protection location from pumping liquid zone extract Body；Inclined isolation baffle plate is provided with above isolating strainer, one end of the isolation baffle plate is fixed on the inner wall of scrubbing tower On, the other end is free end and is tilted to the spray liquid zone, for will elute the silicon powder-containing chlorosilane liquid to get off in scrubbing tower Body water conservancy diversion enters the spray liquid zone, and the silicon powder-containing chlorosilane liquid produced for entering spray liquid zone enters pumping after isolating strainer filters Liquid zone.
Optionally, the top of the isolating strainer is equipped with overflow port, reaches predeterminated position for the liquid level in spray liquid zone When, pumping liquid zone is entered by the overflow port.
Optionally, the outlet of the scrubbing tower circulating pump also backwashes the pump of pipeline and wash tower bottoms by isolating strainer Drawing liquid area is connected, and control valve is provided on the isolating strainer backwash pipeline, is used to reach pre- in the liquid level of spray liquid zone If position, and the liquid level of pumping liquid zone declines, and when scrubbing tower pump operating cycle is normal, opens, with defeated using scrubbing tower circulating pump The chlorosilane liquid produced after supercharged gone out backwashes isolating strainer.
Optionally, the dust removing units include the second differential pressure indicator, the second control unit and two dedusters, and described two are removed Dirt device is connected in parallel, and one opens one standby, and second differential pressure indicator is connect with the entrance and exit of two dedusters respectively, for surveying The front and back pressure difference of deduster in operating status is measured, second control unit is used to be more than in the measured value of the second differential pressure indicator Deduster in operating status is cut off when 0.1MPa, while the deduster in stand-by state is switched to operating status.
Optionally, the multistage cooling unit includes aerial cooler and freon cooler, and the aerial cooler is adopted With eight, for carrying out cooling treatment to the fixed gas after dedusting, by most of chlorosilane condensate in the fixed gas after dedusting Get off and be sent to chlorosilane condensate liquid collecting tank, while exporting remaining fixed gas to freon cooler；The freon cooling Device is used to carry out cooling treatment to the remaining fixed gas, remaining chlorosilane condensate in the remaining fixed gas is got off and sent Toward chlorosilane condensate liquid collecting tank, while exporting and containing impurity hydrogen.
Optionally, the multistage cooling unit further includes cold and hot Jie between aerial cooler and freon cooler Matter heat exchanger, the residue for being used to export aerial cooler using the cold containing impurity hydrogen of freon cooler output Fixed gas carries out cooling treatment, and the chlorosilane condensed out during cooling treatment is sent to chlorosilane condensate liquid collecting tank.
Optionally, the processing unit further includes the first delivery pump, is used for the chlorine silicon in chlorosilane condensate liquid collecting tank The two level spray port through scrubbing tower top, which is sent into inside scrubbing tower, after the supercharging of alkane condensate liquid participates in elution work.
Advantageous effect：
The processing unit of polycrystalline silicon reduction exhaust of the present invention, can be the case where ensureing the hydrogen quality isolated Under, the silica flour that tail gas is brought into will be restored and be effectively treated, the processing energy consumption of reduction tail gas is greatly lowered, at reduction tail gas Reason device equipment amount substantially reduce, reduce system overhaul, maintenance difficulty, additionally it is possible to throwing is greatly decreased when new spectra is built Amount is provided, higher economic benefit is created for enterprise.
Description of the drawings
Fig. 1 is the structural schematic diagram of the processing unit of polycrystalline silicon reduction exhaust provided in an embodiment of the present invention；
Fig. 2 is the structural schematic diagram of scrubbing tower circulating pump protection location in Fig. 1；
Fig. 3 is the structural schematic diagram of scrubbing tower in Fig. 1；
Fig. 4 is the structural schematic diagram of active carbon adsorption column in Fig. 1.
In figure：1- restores tail gas；2- scrubbing towers；3- scrubbing tower slag-drip openings；4- scrubbing tower circulating pumps；5- dedusting lists Member；6- aerial coolers；The cold and hot media heat exchangers of 7-；8- freon coolers；9- liquid freon entrances；10- gaseous states Freon exports；The first delivery pumps of 11-；12- chlorosilane condensate liquid collecting tanks；13- chlorosilane storage tanks；14- second is conveyed Pump；15- rectification working processes；16- hydrogen gas compressors；17-7 DEG C of water- to-water heat exchanger；The 18-7 DEG C of mouth of a river waterborne；19-7 DEG C of water return water Mouthful；20- first order active carbon adsorption columns；The second level 21- active carbon adsorption column；22- third level active carbon adsorption columns；23- Fourth stage active carbon adsorption column；24- adsorption column regeneration purge hydrogen inlets；25- adsorption column regeneration purge hydrogen outlets；26- 7 DEG C of water inlets；27-7 DEG C of water out；28-1.2MPa saturated vapor entrance；29-1.2MPa saturated vapor condensate outlet； 30- steam traps；31- hydrogen gas buffers；32- restores process；33- silicon powder-containing chlorosilane liquid produceds；34- ceramic elements； 35- ceramic filters；36- backwash ceramic element slag-drip openings；The first differential pressure indicators of 37-；38- liquid-level switch tanks；39- liquid levels Switch；40- pressure gauges；41- backwash ceramic element clean-up lines；42- isolating strainers backwash pipeline；43- isolating strainers； 44- isolation baffle plates；45- circulating pump protection locations；46- level-one spray ports；47- two level spray ports；48- fixed gases；49- Fixed gas after dedusting；Fixed gas after 50- is air-cooled；The fixed gas to cool down after 51- heat exchange；52- freon is after cooling to be contained There is impurity hydrogen；What is heated up after 53- heat exchange contains impurity hydrogen；Contain impurity hydrogen after 54- boostings；Contain after 55- coolings Impurity hydrogen；56- pure hydrogens.
Specific implementation mode
To make those skilled in the art more fully understand technical scheme of the present invention, with reference to the accompanying drawings and examples to this Invention is described in further detail.
The embodiment of the present invention provides a kind of processing unit of polycrystalline silicon reduction exhaust, relates generally to production of polysilicon technical staff The application of the research of skill and device in production of polysilicon.The temperature of the reduction tail gas is 130 DEG C or so, and pressure is 0.45MPa comprising hydrogen, chlorosilane and a small amount of silica flour gaseous mixture, the chlorosilane include trichlorosilane, silicon tetrachloride and Dichlorosilane.Wherein, percent by volume of the silica flour in restoring tail gas is only 0.1%, although accounting is small, to polysilicon Production technology is affected, it should be removed；Certainly, can also contain in the gaseous mixture a small amount of HCl (hydrogen chloride) and PH3Impurity such as (hydrogen phosphide).
It should be noted that " a small amount of " that occurs in the present invention refers to that content is few, in the art it is generally acknowledged that HCl Percent by volume be less than 0.1%, PH3Percent by volume just belong to a small amount of scope less than 50PPM.Occur in the present invention " left and right " refers to adding and subtracting the unit of preset quantity, such as 130 DEG C or so in basic value, it is assumed that the unit of preset quantity is 5 A unit then refers to 125 DEG C~135 DEG C, in other words, refers to 130 DEG C of ± first preset temperature values；Such as 85% is left again It is right, it is assumed that the unit of preset quantity is 3 units, then refers to 82%~88%, in other words, refers to that 85% ± the first is default Percentage.As for the unit of the corresponding preset quantity of each numerical value, can be set according to actual conditions by those skilled in the art.
As shown in Figure 1, the processing unit includes：
Scrubbing tower 2, for being carried out at elution to the reduction tail gas 1 using top-down chlorosilane leacheate in tower Reason, and from tower reactor output silicon powder-containing chlorosilane liquid produced 33, fixed gas 48 is exported from tower top；The silicon powder-containing chlorosilane liquid produced 33 wraps Include the mixed liquor of silica flour and chlorosilane, and a small amount of impurity (such as HCl, PH3)；The fixed gas 48 includes hydrogen, is not absorbed Chlorosilane and silica flour gaseous mixture, and a small amount of impurity (such as HCl, PH3)；
Circulating pump protection location 45, the silica flour in silicon powder-containing chlorosilane liquid produced 33 for removing the output of 2 tower reactor of scrubbing tower With chlorosilane liquid produced is exported after impurity, silica flour and impurity, as purer liquid chlorine are practically free of in the chlorosilane liquid produced Silane；
Scrubbing tower circulating pump 4, through scrubbing tower 2 after the chlorosilane liquid produced supercharging for exporting circulating pump protection location 45 The level-one spray port 46 in portion is sent into 2 inside of scrubbing tower as leacheate and participates in elution work；
Dust removing units 5, the silica flour in fixed gas 48 for removing the output of 2 tower top of scrubbing tower, obtain not coagulating after dedusting Gas 49；Fixed gas 49 since silica flour is removed by dust removing units 5, therefore after the dedusting includes hydrogen and unabsorbed chlorine silicon The gaseous mixture of alkane, and a small amount of impurity (such as HCl, PH3)；
Multistage cooling unit, for making the fixed gas 49 after dedusting pass through multistage cooling treatment successively, by after dedusting not Chlorosilane in solidifying gas 49 all condenses out and is sent to chlorosilane condensate liquid collecting tank 12, while exporting and containing a small amount of impurity (such as HCl, PH3, chlorosilane) hydrogen；
Multistage activated carbon adsorption unit, for making the hydrogen containing a small amount of impurity of multistage cooling unit output pass through successively The impurity mixed in hydrogen is all removed, obtains pure hydrogen 56 and be sent to hydrogen gas buffer 31 by multi-stage absorption processing.
In the present embodiment, to prevent the amount for entering the chlorosilane leacheate in scrubbing tower 2 excessive, scrubbing tower can be recycled It is sent to chlorine silicon in part in the chlorosilane liquid produced after supercharged of 4 output of pump other than being sent into inside scrubbing tower through level-one spray port Alkane storage tank 13；It is also possible to which the chlorosilane condensate liquid in chlorosilane condensate liquid collecting tank 12 is sent to chlorosilane storage tank 13.And Liquid chlorosilane in chlorosilane storage tank 13 can be delivered to the rectification working process 15 in downstream by the second delivery pump 14, be filled using rectifying Setting can reuse after carrying out separating treatment to dichlorosilane, trichlorosilane and silicon tetrachloride.In addition, hydrogen gas buffer Purified hydrogen in 31 can transport to the reduction process 32 of upstream, and pure hydrogen is made to participate in reduction reaction in reduction apparatus, To produce electronic-grade polycrystalline silicon.Wherein, the pressure limit of the liquid chlorosilanes of the second delivery pump 14 output is 1.0~1.5MPa.
As it can be seen that the processing by aforementioned device, the silica flour restored in tail gas 1 can either be effectively removed (utilize dedusting list Member and circulating pump protection location are realized), and the hydrogen in tail gas and chlorosilane good separation can will be restored, and the hydrogen isolated The purified hydrogen obtained after multistage activated carbon adsorption unit adsorption treatment can send to upstream reduction process and participate in reduction reaction；Point The chlorosilane (including chlorosilane condensate liquid and chlorosilane liquid produced) separated out can be sent to downstream rectification working process, be repeated after separating treatment It utilizes.Moreover, the equipment amount for participating in processing is seldom, energy consumption is relatively low, so production cost and maintenance, maintenance cost are relatively low.
As shown in Fig. 2, the circulating pump protection location 45 (does not show including the first differential pressure indicator 37, the first control unit in figure Go out) and two ceramic filters 35, two ceramic filters 35 be connected in parallel, and one opens one standby, i.e., one in operation State, another is in stand-by state.
The ceramic filter 35 is internally provided with accurate ceramic element, being capable of effectively 2 tower reactor output of filtration washing tower Silicon powder-containing chlorosilane liquid produced 33 in 99% or more granularity be more than the silica flour and impurity of 1 μm (or be more than 1300 mesh), from washing The silicon powder-containing chlorosilane liquid produced 33 of 2 tower reactor of tower output enters from the lower part of ceramic filter 35 in operating status, from lower On after the filtration treatment of ceramic element 34, export purer chlorosilane liquid produced from the top of ceramic filter 35, then send to Scrubbing tower circulating pump 4 carries out increase processing, to the even running of the scrubbing tower circulating pump 4 of effective protection, avoids impurity pair The abrasion of pump.
First differential pressure indicator 37 is connect with the entrance and exit of two ceramic filters 35 respectively, that is, is arranged and is made pottery at two Before and after porcelain filter 35, the front and back pressure difference for measuring ceramic filter 35 in operating status, first control unit Ceramic filter 35 in operating status is cut off when being more than 0.1MPa for the measured value in the first differential pressure indicator 37, simultaneously will Ceramic filter 35 in stand-by state is switched to operating status, to switch off the ceramic filter 35 of operation in time, keeps away Exempt from that the working media throughput caused by resistance is excessive is low, triggering interlocking, and the phenomenon that cause scrubbing tower 4 stop jumping of circulating pump Occur.
After ceramic filter 35 in operating status is removed (i.e. switching isolation), in order to make it meet stand-by state Required condition, to revert to stand-by state, as shown in Fig. 2, can utilize the first delivery pump 11 that chlorosilane condensate liquid is made to collect Part chlorosilane condensate liquid in tank 12 enters the top rinse mouth of ceramic filter 35 through backwash ceramic element clean-up line 41, Ceramic element 34 is backwashed from top to bottom, the chlorosilane liquid produced rich in silica flour formed after flushing is through ceramic filter 35 The backwash ceramic element slag-drip opening 36 of bottom is sent to the slurry treatment process (not shown) in downstream.
In addition, the circulating pump protection location 45 further includes liquid-level switch tank 38, respectively with two ceramic filters 35 Outlet connected with the entrance of scrubbing tower circulating pump 4, that is, after being located at two ceramic filters 35, before scrubbing tower circulating pump 4.
Level chain can be arranged to scrubbing tower circulating pump 4 to protect, keep scrubbing tower circulating pump 4 low with liquid-level switch tank 38 Level chain.Specifically, it is provided with liquid-level switch 39 on liquid-level switch tank 38, for measuring the liquid level in liquid-level switch tank 38, First control unit stops the interlocking of scrubbing tower circulating pump 4 when being additionally operable to the liquid level in liquid-level switch tank 38 less than 70% Vehicle avoids causing pump overheat to burn out because of liquid level deficiency to the safe operation of effective protection pump.
Can also pressure interlock protection be set to scrubbing tower circulating pump 4, make in scrubbing tower circulating pump 4 and liquid-level switch tank 38 Fluid pressure teletransmission interlocking.Specifically, it is additionally provided with pressure gauge 40 on the liquid-level switch tank 38, for measuring liquid-level switch Fluid pressure in tank 38, when first control unit is additionally operable to the fluid pressure in liquid-level switch tank 38 less than 0.1MPa Make 4 interlock shutdown of scrubbing tower circulating pump, to the safe operation of effective protection pump, avoids causing pump overheat to be burnt because of liquid level deficiency It is bad.
In the present embodiment, circulating pump protection location 45 is the fluid rich in impurity, and the pump housing pair mainly for working media The more demanding situation of working media, since scrubbing tower circulating pump 4 all uses canned motor pump, silica flour too high levels meeting under normal circumstances Larger abrasion is caused to canned motor pump, therefore is applicable in this equipment.Specifically, pass through the ceramic filter in circulating pump protection location 45 35 effectively remove the silica flour and impurity in the silicon powder-containing chlorosilane liquid produced 33 of 2 tower reactor of scrubbing tower output, to be recycled to scrubbing tower Pump 4 is protected, and the liquid chlorosilane abrasion pump rich in silica flour is avoided.
It is well known that the density of silicon is 2.33g/cm3, the averag density of chlorosilane is 1.4g/cm3, it is seen then that the density of silicon More than the averag density of chlorosilane.Therefore, in the scrubbing tower 2 using top-down chlorosilane leacheate to reduction tail gas 1 into After row elution, the chlorosilane liquid produced of silicon powder-containing can sink to rapidly wash tower bottoms, be easier to detach with fixed gas.
Moreover, again through washing after the chlorosilane liquid produced supercharging that scrubbing tower circulating pump 4 exports circulating pump protection location 45 2 inside of the feeding of level-one spray port 46 scrubbing tower for washing 2 top of tower participates in elution work as leacheate, can will restore in tail gas 80% or so silica flour spray washing gets off, then by interval deslagging, can will save bit by bit in 2 bottom of scrubbing tower rich in silica flour The slurry process (not shown) that chlorosilane liquid produced is delivered to downstream is handled；Chlorosilane leacheate to reduction tail gas into While row elution, cold also is had input to reduction tail gas, reduction tail gas is made to be cooled down during elution.
As shown in figure 3, the bottom of the scrubbing tower 2 is provided with vertical isolating strainer 43, it is used for the bottom in scrubbing tower Portion region is separated into spray liquid zone (region for being located at 43 left side of isolating strainer in Fig. 2) and pumping liquid zone (is located in Fig. 2 and filter is isolated The region on 43 right side of net), and scrubbing tower circulating pump 4 extracts liquid through circulating pump protection location 45 from the pumping liquid zone；Every Top from strainer 43 is provided with inclined isolation baffle plate 44, and one end of the isolation baffle plate 44 is fixed on the inner wall of scrubbing tower 2 On, the other end is free end and is tilted to the spray liquid zone that angle of inclination is to press from both sides 40 ° of angles with horizontal plane, for that will wash The silicon powder-containing chlorosilane liquid produced water conservancy diversion eluted in tower 2 enters the spray liquid zone, and enters the silicon powder-containing chlorine silicon of spray liquid zone Alkane liquid enters pumping liquid zone after the filtering of isolating strainer 43.The bottom of spray liquid zone and pumping liquid zone is designed with scrubbing tower deslagging The chlorosilane liquid produced rich in silica flour that the two areas are saved bit by bit, can be delivered to the slurry process in downstream by mouth 3 by regular deslagging.
The isolating strainer 43 is the strainer of 60 mesh of multilayer, to make in the silicon powder-containing chlorosilane liquid produced in spray liquid zone absolutely After silicon powder particle filtering of the most diameter more than 0.3mm, pumping liquid zone is entered back into, it can be by this field skill as the specific number of plies Art personnel determine according to actual conditions.
The top of the isolating strainer 43 is equipped with overflow port (not shown), reaches pre- for the liquid level in spray liquid zone If when position, entering pumping liquid zone by the overflow port, lead to pump depletion to avoid because pumping liquid zone lacks liquid.Certainly, described The height of overflow port bottom is flushed with the height of the predeterminated position.The predeterminated position can be the 80% of spray liquid area height At position, that is, spray liquid zone liquid level reach 80% after, pumping liquid zone will be entered by 43 top overflow port of isolating strainer.
The outlet of the scrubbing tower circulating pump 4 also backwashes the pumping of pipeline 42 and 2 bottom of scrubbing tower by isolating strainer Liquid zone is connected, and control valve is provided on the isolating strainer backwash pipeline 42, when the liquid level of spray liquid zone reaches predeterminated position (can be at 80% position of spray liquid area height), and the liquid level of pumping liquid zone declines, and the operation of scrubbing tower circulating pump 4 is just Often, illustrate that silica flour clogging occurs in isolating strainer 43, opening control valve at this time makes isolating strainer backwash pipeline 42 be connected, just The chlorosilane liquid produced after supercharged exported using scrubbing tower circulating pump 4 backwashes isolating strainer 43, to wash out isolation Silica flour on strainer 43.
Through foregoing description it is found that scrubbing tower circulating pump 4 export chlorosilane liquid produced after supercharged (pressure limit be 1.0~ 1.5MPa) it is segmented into three parts, the parts respectively A1, the parts A2 and the parts A3 (as shown in Figure 1).Wherein, the parts A1 pass through Isolating strainer backwashes the pumping liquid zone that pipeline 42 enters 2 bottom of scrubbing tower, this part is only when isolating strainer is blocked by silica flour Flow controllable when just opening and come into operation, and coming into operation is 10 ton hours, after the clogging of isolating strainer is eliminated, you can It closes；The parts A2 enter chlorosilane storage tank 13, and the flow of this part is controllable to 130 ton hours；On the washed tower in the parts A3 2 The level-one spray port 46 in portion enters scrubbing tower 2, and the flow of this part can be adjusted according to production of polysilicon operating mode, regular situation Under may be set to 100 ton hours.
In the present embodiment, the dust removing units 5, which are used to restore in tail gas, is not washed silica flour that tower 2 washs into one Step effectively removes comprising and the second differential pressure indicator, the second control unit and two dedusters, two dedusters are connected in parallel, And one opens one standby, i.e., one is in operating status, and another is in stand-by state.
The deduster is internally provided with the stainless steel mesh filter core (i.e. fine and close steel wire cylinder) of tubular, can effectively cross diafiltration In the fixed gas 48 of 2 tower top of tower output 99.5% or more the silica flour more than 1000 mesh is washed, while can will be carried secretly in the fixed gas Drop keep off cutting down together and, enter from the fixed gas 48 that 2 tower top of scrubbing tower exports from deduster lower part in operating status, From bottom to top after the filtration treatment of deduster, the fixed gas 49 after dedusting, silicon wherein included are exported from the top of deduster Powder content few (0.5% or less), grain size are minimum, it is thus possible to ensure that subsequent handling production is normal.
Second differential pressure indicator is connect with the entrance and exit of two dedusters respectively, in operating status for measuring The front and back pressure difference of deduster, second control unit are used to that fortune will to be in when the measured value of the second differential pressure indicator is more than 0.1MPa The deduster of row state is cut off, while the deduster in stand-by state is switched to operating status.
After deduster in operating status is removed (i.e. switching isolation), in order to make it meet item needed for stand-by state Part can utilize the first delivery pump 11 to make the part chlorine silicon in chlorosilane condensate liquid collecting tank 12 to revert to stand-by state Alkane condensate liquid enters the top rinse mouth of deduster, backwashes to the filter core of deduster, is formed after flushing from top to bottom Carry silica flour chlorosilane liquid produced (its compared to the silicon powder-containing chlorosilane liquid produced 33 that 2 tower reactor of scrubbing tower exports, silica flour content is few It can very much) send to scrubbing tower 2 and recycle.
As shown in Figure 1, the first delivery pump 11 can be additionally used in the chlorosilane condensate liquid in chlorosilane condensate liquid collecting tank 12 Two level spray port 47 through scrubbing tower top is sent into inside scrubbing tower after supercharging participates in elution work as leacheate, for prevent into The amount for entering the chlorosilane leacheate in scrubbing tower 2 is excessive, and the part chlorosilane in chlorosilane condensate liquid collecting tank 12 can be made cold Lime set is sent into inside scrubbing tower 2, and another part chlorosilane condensate liquid is sent into chlorosilane storage tank 13, rest part chlorosilane condensate liquid Return to chlorosilane condensate liquid collecting tank 12.
In the present embodiment, (part) chlorosilane liquid produced that scrubbing tower circulating pump 4 exports circulating pump protection location 45 is pressurized The level-one spray port 46 on 2 top of washed tower is sent into inside scrubbing tower 2 again afterwards, and the first delivery pump 11 collects chlorosilane condensate liquid The two level spray port 47 on 2 top of washed tower is sent into scrubbing tower 2 again after (part) chlorosilane condensate liquid increase that tank 12 exports Portion makes the chlorosilane of this two parts liquid participate in elution work as leacheate, to restore in tail gas 95% or so silicon Powder spray washing gets off, and only 5% or so silica flour is exported as fixed gas from 2 tower top of scrubbing tower, while being restored in tail gas 60% chlorosilane is leached, and is exported from 2 tower reactor of scrubbing tower after being mixed into leacheate.Moreover, from 46 He of level-one spray port Two level spray port 47 enters the leacheate of scrubbing tower 2 while being eluted to reduction tail gas, is also had input to reduction tail gas Cold makes reduction tail gas be down to 70 DEG C or so by 130 DEG C or so in scrubbing tower, therefore the fixed gas 48 of 2 tower top of scrubbing tower output The temperature of fixed gas 49 after the dedusting exported with dust removing units 5 is 70 DEG C or so.As can be seen that two level spray is sprayed in level-one Cold supplement is carried out to reduction tail gas on the basis of leaching, if two level spray is not provided with, in contrast, from 2 tower top of scrubbing tower The temperature of the fixed gas of output can rise, to increase the load of aerial cooler 6 and freon cooler 8.
As shown in Figure 1, the multistage cooling unit includes aerial cooler 6 and freon cooler 8, the air cooling Device 6 uses eight, provides power by the wind turbine of its underpart and provides cold using air, is removed for being 70 DEG C or so to temperature Fixed gas 49 after dirt carries out cooling treatment, will be under most of chlorosilane (85% or so) condensation in the fixed gas 49 after dedusting Carry out and be sent to chlorosilane condensate liquid collecting tank 12, while the remaining fixed gas that output temperature is 40 DEG C or so is to freon cooler 8, therefore aerial cooler 6 provides 85% or so cold for the condensation process of the fixed gas 49 after dedusting.The freon cooling Device 8 is used to carry out cooling treatment (i.e. subzero treatment) to the remaining fixed gas, by its chlorine residue silicon in the remaining fixed gas Alkane (15% or so) condenses out and is sent to chlorosilane condensate liquid collecting tank 12, while exporting and containing impurity hydrogen, wherein there are about 99.8% hydrogen only contains a small amount of chlorosilane, HCl and PH3Equal impurity, therefore freon cooler 8 is not coagulating after dedusting The condensation process of gas 49 provides 15% or so cold.Enter as shown in Figure 1, being additionally provided with liquid freon on freon cooler 8 Mouthfuls 9 and gaseous state freon outlet 10, it is and described after the liquid freon of low temperature enters freon cooler 8 by the entrance 9 Remaining fixed gas exchanges heat, and cold is become gaseous state freon and defeated from the outlet 10 after being utilized by the remaining fixed gas Go out.
Energy-saving fully to recycle cold, after aerial cooler 6, before freon cooler 8, setting one is cold and hot Media heat exchanger 7 can exchange heat the gas that the gas that aerial cooler 6 exports is exported with freon cooler 8.Cause This, more preferably, the multistage cooling unit further includes the cold and hot medium between aerial cooler 6 and freon cooler 8 Heat exchanger 7, the sky for being used to export aerial cooler 6 using the cold containing impurity hydrogen that freon cooler 8 exports Fixed gas after cold carries out cooling treatment, and the chlorosilane condensed out during cooling treatment is sent to chlorosilane condensate liquid and is received Collect tank 12.
Specifically, it is defeated after the fixed gas 49 after the dedusting that aerial cooler 6 is 70 DEG C or so to temperature carries out cooling treatment It is tube side of the fixed gas 50 after 40 DEG C or so air-cooled to cold and hot media heat exchanger 7 to go out temperature, while by 85% or so chlorine Silane condenses out；The cold for the gas that cold and hot media heat exchanger 7 is exported using freon cooler 8 is to the fixed gas after air-cooled 50 are exchanged heat (cooling) processing, the fixed gas 51 to cool down after being -10 DEG C or so of heat exchange from its tube side output temperature to fluorine profit High cooler 8, while part chlorosilane is condensed out again, the chlorosilane that cold and hot media heat exchanger 7 condenses out is compared to air Cooler 6 and freon cooler 8 are many less；The fixed gas 51 to cool down after 8 heat exchanging of freon cooler carries out at deep cooling After reason, 15% or so chlorosilane condensate is got off, 99.8% chlorosilane has been condensed in the fixed gas 49 after dedusting at this time Get off, the freon that then output temperature is -44 DEG C or so is after cooling to contain impurity hydrogen 52 to cold and hot media heat exchanger 7 Shell side；Freon is after cooling exchange heat in cold and hot media heat exchanger 7 containing impurity hydrogen 52 after form 10 DEG C or so of heat exchange What is heated up afterwards exports containing impurity hydrogen 53 and from the shell side of cold and hot media heat exchanger 7.And aerial cooler 6, cold and hot medium change The chlorosilane condensate liquid that hot device 7 and freon cooler 8 condense out is sent into chlorosilane condensate liquid collecting tank 12.
Through foregoing description it is found that the chlorosilane that exports after the supercharging of the first delivery pump 11 of chlorosilane condensate liquid collecting tank 12 is cold Lime set (pressure limit be 1.0~1.5MPa) is segmented into five parts, the parts respectively B1, the parts B2, the parts B3, the parts B4 and The parts B5 (as shown in Figure 1).Wherein, the parts B1 enter chlorosilane storage tank 13, and liquid level of this part for chlorosilane storage tank 13 is flat Weighing apparatus, flow should be controlled in 40 ton hours, and actually this part can be closed；The two level on washed 2 top of tower in the parts B2 is sprayed Drench mouth 47 enter scrubbing tower 2, with realize two level spray, and bring into scrubbing tower 2 the second low-temperature receiver (the first low-temperature receiver be level-one spray Leaching), flow should be controlled in 40 ton hours；The parts B3 return to chlorosilane condensate liquid collecting tank 12, and pipeline is spare where this part Pipeline can not have under normal circumstances；The parts B4 enter the top rinse mouth of the removed deduster in dust removing units 5, this Flow controllable when partly only just opening and comes into operation after deduster is removed, and coming into operation is 10 ton hours, once be removed After deduster reverts to stand-by state, you can close；The parts B5 enter the top rinse mouth of removed ceramic filter 35, this Flow controllable when partly only just opening and comes into operation after ceramic filter is removed, and coming into operation is 10 ton hours, once by cutting After the ceramic filter removed reverts to stand-by state, you can close.
As shown in Figure 1, (what is heated up after i.e. aforementioned heat exchange contains impurities H to the impurity hydrogen that contains of multistage cooling unit output Gas 53) before entering multistage activated carbon adsorption unit, in order to preferably meet the job requirement of active carbon adsorption column to obtain Better adsorption effect can make the place that hydrogen gas compressor 16 and liquid medium heat exchanger are first passed through containing impurity hydrogen Reason.Therefore, more preferably, the processing unit further includes hydrogen gas compressor 16 and liquid medium heat exchanger, the hydrogen gas compressor 16 containing impurity hydrogen to described for carrying out compression pressure-raising, and impurity hydrogen 54 is contained after being boosted；The liquid medium changes Hot device is used to carry out cooling treatment to containing impurity hydrogen 54 after the boosting, impurity hydrogen 55 is contained after being cooled down, then Multistage activated carbon adsorption unit will be sent into containing impurity hydrogen 55 carry out adsorption treatment after the cooling again.
Wherein, 7 DEG C of water- to-water heat exchangers 17 can be used in liquid medium heat exchanger.As shown in Figure 1, also being set on 7 DEG C of water- to-water heat exchangers 17 There are 7 DEG C of mouths of a river 18 waterborne and 7 DEG C of water water return outlets 19.
Specifically, it (heats up after i.e. aforementioned heat exchange containing impurity hydrogen from described in the output of the shell side of cold and hot media heat exchanger 7 Contain impurity hydrogen 53) temperature be 10 DEG C or so, pressure 0.45MPa, the compression pressure-raising through hydrogen gas compressor 16, by it Pressure is carried to 1.8MPa, temperature also due to compression and the recirculated water that rises, while being carried by hydrogen gas compressor 16 exchanges heat Device is cooled to 30 DEG C or so, to obtain containing impurity hydrogen 54 after the boosting that temperature is 30 DEG C or so, pressure is 1.8MPa.Institute It states after boosting containing cooling treatment of the impurity hydrogen 54 through 7 DEG C of water- to-water heat exchangers 17, obtains that temperature is 10 DEG C or so, pressure is Contain impurity hydrogen 55 after the cooling of 1.8MPa.
As shown in Figure 1, in the present embodiment, the multistage activated carbon adsorption unit includes concatenated level Four activated carbon adsorption Column, respectively first order active carbon adsorption column 20, second level active carbon adsorption column 21, third level active carbon adsorption column 22 and the 4th Grade active carbon adsorption column 24.Wherein, every grade of active carbon adsorption column includes two active carbon adsorption columns, and one open it is one standby, i.e., one A in operating status, another is in stand-by state.Specifically, the processing unit further includes timing unit and third control Unit, the timing unit is for measuring active carbon adsorption column cumulative operation time in operating status, the third control Unit is used to be cut off when active carbon adsorption column cumulative activation in operating status full 12 is small, while will be in spare shape The active carbon adsorption column of state is switched to operating status, to realize that automatically switching spare active carbon adsorption column is in working condition, To ensure that adsorption process is efficient, be carried out continuously.
Active carbon adsorption column in operating status is avoided putting because what adsorption process occurred to ensure adsorption effect Thermal response is highly exothermic and makes activated carbon temperature rapid increase, causes adsorption effect to be deteriorated, enters work in active carbon adsorption column Before stage, the temperature of activated carbon is down to 10 DEG C or so using 7 DEG C of water and (is contained after into the cooling of multistage activated carbon adsorption unit It is also 10 DEG C or so to have the temperature of impurity hydrogen 55), and 7 DEG C of water are continually fed into the working stage of active carbon adsorption column, with band Walk the heat of adsorption process generation.Specifically, the lower part of active carbon adsorption column is equipped with 7 DEG C of water inlets 26, top goes out equipped with 7 DEG C of water Mouth 27 opens the valve on 7 DEG C of water inlets 26 and 7 DEG C of 27 place pipelines of water out, is passed through 7 to active carbon adsorption column from bottom to top DEG C water, can take away the heat generated due to adsorption reaction in active carbon adsorption column, and from the 7 of active carbon adsorption column top DEG C water out 27 is sent out, so as not to active carbon adsorption column heat up during the work time it is too fast.
It is spare to revert in order to make it meet condition needed for stand-by state for removed active carbon adsorption column State needs to carry out regeneration treatment to it.Specifically, the top of active carbon adsorption column is equipped with the suction being connected with hydrogen gas buffer 31 Attached column regeneration purge hydrogen inlet 24, bottom are equipped with the absorption being connected with the hydrogen in downstream recovery processing process (not shown) Column regeneration purges hydrogen outlet 25, and the top of active carbon adsorption column is equipped with 1.2MPa saturated vapors entrance 28, lower part is equipped with 1.2MPa saturated vapors condensate outlet 29 closes 7 DEG C of water inlets 26 and 7 DEG C of water outs 27 when needing to carry out regeneration treatment Valve on the pipeline of place opens 1.2MPa saturated vapors entrance 28 and 29 place pipeline of 1.2MPa saturated vapors condensate outlet On valve, 1.2MPa saturated vapors are passed through to the active carbon adsorption column in reproduced state from top to bottom, by activated carbon adsorption The pressure of column carries out heating regeneration to 0.05MPa, and by the heat of saturated vapor by 1.8MPa pressure releases to active carbon adsorption column, Make a small amount of impurity (such as chlorosilane, HCl, PH adsorbed thereon3) heated, these impurity can take off after absorbing enough heats From active carbon adsorption column, at the same time need to open on hydrogen gas buffer 31 to the pipeline of adsorption column regeneration purge hydrogen inlet 24 Valve on valve and adsorption column regeneration purge hydrogen outlet 25 to hydrogen recovery processing process pipeline, utilizes hydrogen gas buffer The hydrogen stored in 31 from top to bottom purges active carbon adsorption column, and the control of purging amount is in 500Nm3/ h, make departing from The impurity of active carbon adsorption column is recycled process with the hydrogen that purging hydrogen enters downstream.
The adsorption treatment for passing through aforementioned level Four active carbon adsorption column successively, has effectively removed hydrogen and (has contained after i.e. aforementioned cooling Have impurity hydrogen 55) in a small amount of chlorosilane, HCl and physical property and HCl it is very much like and the polycrystalline of production can be caused The PH of silicon quality decline3, and more pure pure hydrogen 56 is obtained, to ensure that the quality of hydrogen, meet downstream reduction work Sequence 32 produces electronic-grade polycrystalline silicon.
In the following, by taking annual output is 30,000 tons of polycrystalline process units as an example, it is described in detail at reduction tail gas described in the present embodiment Manage the technological process of device：
One, washing tail gas tower section is restored
Autoreduction device output pressure be 0.5MPa, the reduction tail gas that temperature is 130 DEG C or so, wherein containing 9.4 tons/ Hour hydrogen, 68 ton hour silicon tetrachlorides, 88.4 ton hour trichlorosilanes, the gaseous mixture of 13.6 ton hour dichlorosilanes, Total amount is 179.4 ton hours.
Tail gas is restored from 2 lower part of scrubbing tower to enter, it is defeated by the level-one spray washing of scrubbing tower circulating pump 4 and first The two level spray washing for sending pump 11 removes the silica flour for restoring in tail gas 95% in scrubbing tower 2, and will restore in tail gas 60% chlorosilane elutes, and is mixed into spray liquid, while the temperature for restoring tail gas is down to 70 DEG C or so, is exported from tower top Fixed gas 48, and enter dust removing units 5.
The temperature exported from 2 tower top of scrubbing tower is that 70 DEG C or so of fixed gas 48 enters dust removing units, in dust removing units The silica flour not being washed down in fixed gas 48 is further effectively removed in deduster, is more than 1000 purposes by 99.5% or more Silica flour is removed.
Scrubbing tower circulating pump 4 extracts silicon powder-containing chlorosilane liquid produced 33 from 2 bottom of scrubbing tower, and silicon powder-containing chlorosilane liquid produced 33 is first Into ceramic filter 35, use accurate ceramic element 34, can effectively filter 99% or more 1 μm of granularity > it is (or big In 1300 mesh) impurity；Filtered chlorosilane liquid produced from ceramic filter 35 come out after enter liquid-level switch tank 38, then into Enter scrubbing tower circulating pump 4, after pumping pressure-raising, the level-one spray port 46 on 2 top of washed tower enters in scrubbing tower 2 to restoring tail gas Carry out level-one spray washing.According to the level condition in scrubbing tower 2, about 130 ton hours of 4 output of control scrubbing tower circulating pump Chlorosilane liquid produced is produced to chlorosilane storage tank 13.
Chlorosilane condensate liquid collecting tank 12 exports the chlorosilane condensate liquid of 40 ton hours through the first delivery pump 11, by washing The two level spray port 47 for washing 2 top of tower enters in scrubbing tower 2 to reduction tail gas progress two level spray washing.According to chlorosilane condensate The level condition of liquid collecting tank produces the chlorosilane condensate liquid of about 40 ton hours wherein more than needed to chlorosilane storage tank 13.And Chlorosilane liquid produced in chlorosilane storage tank 13 is handled through subsequent rectification working process 15, to dichlorosilane, trichlorosilane and tetrachloro SiClx carries out separation recycling.
Two dedusters one in dust removing units 5 are opened one standby, when pressure difference is more than 0.1MPa before and after deduster, switch in time It is cold from chlorosilane condensate liquid collecting tank 12 to attract chlorosilane after deduster switching isolation by the first delivery pump 11 for deduster Lime set backwashes the filter core of deduster, and the chlorosilane liquid produced for carrying silica flour obtained after flushing is delivered to scrubbing tower 2 Recycling.
The spray liquid zone of 2 bottom of scrubbing tower is periodically opened with the scrubbing tower slag-drip opening 3 of pumping liquid zone bottom, and discharge is rich in silicon The chlorosilane of slag is delivered to downstream slurry treatment process to remove the silica flour deposited.
The bottom of scrubbing tower 2 is fixed with isolating strainer 43, and the bottom section in scrubbing tower is separated into spray liquid zone and pump Drawing liquid area, the top of isolating strainer 43 are provided with the isolation baffle plate 44 of 40 degree of inclination, will the interior silicon powder-containing eluted of scrubbing tower 2 Chlorosilane liquid produced water conservancy diversion enters the spray liquid zone, then the isolating strainer 43 through 60 mesh of multilayer, by most diameter more than 0.3mm's After silicon powder particle filtering, into pumping liquid zone.After the liquid level for spraying liquid zone reaches 80%, it will overflow more than 43 top of isolating strainer Head piece, and pumping liquid zone is overflowed to, it avoids leading to pump depletion because pumping liquid zone lacks liquid.Reach 80% when spraying liquid zone liquid level, And pumping liquid zone liquid level declines, and when pump operation is normal, illustrating isolating strainer 43, there are silica flour cloggings, can open at this time every From the control valve on strainer backwash pipeline 42, the chlorosilane liquid produced after supercharged exported using scrubbing tower circulating pump 4 is to isolation Strainer 43 is backwashed.
Two, cooling, deep cooling part
Fixed gas 49 after the dedusting that the temperature exported from dust removing units 5 is 70 DEG C or so enters eight aerial coolers 6, Cooled down by wind turbine, the temperature of the fixed gas 49 after dedusting is down to 40 DEG C hereinafter, being condensed out in aerial cooler 6 Chlorosilane send into chlorosilane condensate liquid collecting tank 12.
Exported from aerial cooler 6 it is air-cooled after fixed gas 50, enter cold and hot media heat exchanger 7, and go out freon The gas that cooler 8 exports exchanges heat, the fixed gas 51 to cool down after the heat exchange that tube side exports -10 DEG C or so, in cold and hot Jie The chlorosilane condensed out in matter heat exchanger 7 is also sent into chlorosilane condensate liquid collecting tank 12.
The fixed gas 51 to cool down after the heat exchange that 7 tube side of cold and hot media heat exchanger exports enters in freon cooler 8, Heat is absorbed by the freon evaporation of shell side, 51 temperature of gas is down to -44 DEG C or so, to which 99.8% chlorosilane is cold It coagulates, and exports the freon shell side after cooling containing impurity hydrogen 52 to cold and hot media heat exchanger 7, then from cold and hot Jie What is heated up after the shell side output heat exchange of matter heat exchanger 7 contains impurity hydrogen 53, the chlorine silicon condensed out in freon cooler 8 Alkane is also sent into chlorosilane condensate liquid collecting tank 12.The hydrogen of the composition about 99.8% of gas 53 at this time, contains only a small amount of chlorine Silane, HCl and PH3。
Three, compression, cooling segment
The temperature containing impurity hydrogen 53 to heat up after the heat exchange that the shell side of cold and hot media heat exchanger 7 exports is 10 DEG C of left sides The right side, pressure 0.45MPa carry out compression pressure-raising using hydrogen gas compressor 16 then into hydrogen gas compressor 16 to hydrogen 53, will 53 pressure-raising of hydrogen is to 1.8MPa, and due to compression temperature rise, the Heat Exchanger in Circulating Water System carried by compressor cools down hydrogen 53 To 30 DEG C or so, to contain impurity hydrogen 54 after the boosting that output temperature is 30 DEG C or so, pressure is 1.8MPa.
Enter 7 DEG C of water- to-water heat exchangers 17 containing impurity hydrogen 54 after the boosting that hydrogen gas compressor 16 exports, by hydrogen 54 are cooled to 10 DEG C or so.
Four, four level active carbon pressure-variable adsorption
It is 1.8MPa, contains impurity hydrogen 55 after the cooling that temperature is 10 DEG C or so from 7 DEG C of 17 output pressure of water- to-water heat exchanger Enter from 20 bottom of first order active carbon adsorption column, is that 1.8MPa utilizes activated carbon in the environment of temperature is 10 DEG C in pressure Adsorption function is by most chlorosilane and HCl, PH in hydrogen 553Etc. impurity absorptions, then sequentially enter the second level, third Grade, fourth stage active carbon adsorption column.From level Four active carbon adsorption column come out hydrogen, substantially by containing chlorosilane and HCl, PH3Equal impurity almost 100% are removed, and can meet electronic-grade polycrystalline silicon production with the quality of effective guarantee hydrogen.
The more pure pure hydrogen 56 exported from level Four active carbon adsorption column enters hydrogen gas buffer 31, is then fed into The reduction apparatus of trip reduction process is reused.
Inventor has found that the present invention brings following advantageous effect in production of polysilicon：
1) 99.5% silica flour that the reduction tail gas that reduction apparatus generates is brought into can be removed, avoids silica flour abrasion pump, or It causes unit to block, in turn results in system and partially or fully stop.
2) can will restore the power consumption of vent gas treatment by 1.2 ten thousand KWhs/ton of silicon, be down to 0.6 ten thousand KWhs/ton of silicon, save 0.6 ten thousand degree/ 60,000,000 degree of electricity or more are saved in ton silicon, the annual of 10,000 tons production of polysilicon enterprise.
3) newly-built polysilicon enterprise can be made to drop to 100,000,000 yuan hereinafter, dress by 200,000,000 yuan in the investment of reduction exhaust gas processing device It sets total equipment amount and drops to 100 or less by 200.Installation area is by 12000m2Drop to 6000m2Below.
4) operation of reduction exhaust gas processing device, maintenance, maintenance, administrative staff can be down to 35 by original average 60 people Below people.
5) present invention carries out heating regeneration using 1.2MPa saturated vapors to adsorption column, and thermal efficiency higher, heating speed is more Soon, compared with conventional method uses 170 DEG C or so hot water heating regeneration, 15 DEG C can be promoted, regeneration effect is more preferable, has ensured hydrogen Middle PH3Impurity effectively removes, and obtained hydrogen quality disclosure satisfy that electronic-grade polycrystalline silicon produces.Simultaneously because directly using Saturated vapor reduces the setting of heat exchanger, hot-water cylinder, water-delivery pump, reduces about 10,000,000 yuan of equipment investment or more, annual to save 1,000,000 yuan of maintenance cost or more reduces 4 person-times of operating personnel of operation.
6) present invention processing restore tail gas during, need not use Heat Exchanger in Circulating Water System, and 85% cold by Aerial cooler provides, and can save 100 tons of water/hours, and whole year can save 800,000 tons of water, has phase in the area of water resources shortage When big advantage.
7) general overhaul 1 in 2~3 years can be extended to by reduction exhaust gas processing device by annual 1 general overhaul generally taken It is secondary, save 2,000,000 yuan/year of maintenance expense.
In conclusion the present invention produces deficiency existing for CDI devices in polysilicon process for existing improved Siemens, It proposes a kind of novel process device applied to production of polysilicon reduction tail gas, can ensure that the hydrogen quality isolated is full In the case of foot production electronic-grade polycrystalline silicon, the silica flour that tail gas is brought into will be restored and be effectively treated, be greatly lowered and go back protocercal tail The processing energy consumption of gas, by restore vent gas treatment needed for equipment amount substantially reduce, reduce system overhaul, maintenance difficulty, moreover it is possible to It is enough that investment amount is greatly decreased when new spectra is built, create higher economic benefit for enterprise.
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, however the present invention is not limited thereto.For those skilled in the art, in the essence for not departing from the present invention In the case of refreshing and essence, various changes and modifications can be made therein, these variations and modifications are also considered as protection scope of the present invention.

Claims (11)

1. a kind of processing unit of polycrystalline silicon reduction exhaust, the reduction tail gas includes the mixed of hydrogen, chlorosilane and a small amount of silica flour Close gas, which is characterized in that the processing unit includes：
Scrubbing tower, for carrying out elution processing to the reduction tail gas using top-down chlorosilane leacheate in tower, and from Tower reactor exports silicon powder-containing chlorosilane liquid produced, exports fixed gas from tower top, the fixed gas includes hydrogen, unabsorbed chlorosilane With the gaseous mixture of silica flour；
Circulating pump protection location, for remove scrubbing tower tower reactor output silicon powder-containing chlorosilane liquid produced in silica flour and impurity after it is defeated Go out chlorosilane liquid produced；
Scrubbing tower circulating pump, the level-one through scrubbing tower top after the chlorosilane liquid produced supercharging for exporting circulating pump protection location Spray port, which is sent into inside scrubbing tower, participates in elution work；
Dust removing units, the silica flour in fixed gas for removing washing column overhead output, obtain the fixed gas after dedusting；
Multistage cooling unit will be in the fixed gas after dedusting for making the fixed gas after dedusting pass through multistage cooling treatment successively Chlorosilane all condense out and be sent to chlorosilane condensate liquid collecting tank, while exporting and containing impurity hydrogen；
Multistage activated carbon adsorption unit, for making passing through at multi-stage absorption successively containing impurity hydrogen for multistage cooling unit output Reason, obtains pure hydrogen and is sent to hydrogen gas buffer.
2. processing unit according to claim 1, which is characterized in that the circulating pump protection location includes the first pressure difference Table, the first control unit and two ceramic filters, two ceramic filters are connected in parallel, and one open it is one standby, described One differential pressure indicator is connect with the entrance and exit of two ceramic filters respectively, for measuring ceramic filter in operating status Front and back pressure difference, first control unit be used for the first differential pressure indicator measured value be more than 0.1MPa when will be in operating status Ceramic filter excision, while the ceramic filter in stand-by state is switched to operating status.
3. processing unit according to claim 2, which is characterized in that the circulating pump protection location further includes liquid-level switch Tank connect with the entrance of the outlet of two ceramic filters and scrubbing tower circulating pump, liquid is provided on liquid-level switch tank respectively Bit switch, for measuring the liquid level in liquid-level switch tank, first control unit is additionally operable to the liquid level in liquid-level switch tank Make scrubbing tower circulating pump interlock shutdown when less than 70%.
4. processing unit according to claim 3, which is characterized in that it is additionally provided with pressure gauge on the liquid-level switch tank, For measuring the fluid pressure in liquid-level switch tank, first control unit is additionally operable to the fluid pressure in liquid-level switch tank Make scrubbing tower circulating pump interlock shutdown when less than 0.1MPa.
5. according to the processing unit described in any one of claim 1-4, which is characterized in that the bottom of the scrubbing tower is provided with Vertical isolating strainer, for the bottom section in scrubbing tower to be separated into spray liquid zone and pumping liquid zone, and scrubbing tower recycles Pump extracts liquid through circulating pump protection location from the pumping liquid zone；Inclined isolation gear is provided with above isolating strainer One end of plate, the isolation baffle plate is fixed on the inner wall of scrubbing tower, and the other end is free end and is tilted to the spray liquid zone, Enter the spray liquid zone for the silicon powder-containing chlorosilane liquid produced water conservancy diversion to get off will to be eluted in scrubbing tower, and enters containing for spray liquid zone Silica flour chlorosilane liquid produced enters pumping liquid zone after isolating strainer filters.
6. processing unit according to claim 5, which is characterized in that the top of the isolating strainer is equipped with overflow port, uses In when the liquid level for spraying liquid zone reaches predeterminated position, pumping liquid zone is entered by the overflow port.
7. processing unit according to claim 6, which is characterized in that the outlet of the scrubbing tower circulating pump also passes through isolation Strainer backwash pipeline is connected with the pumping liquid zone of wash tower bottoms, and control is provided on the isolating strainer backwash pipeline Valve is used to reach predeterminated position in the liquid level of spray liquid zone, and the liquid level of pumping liquid zone declines, and scrubbing tower pump operating cycle It opens when normal, isolating strainer is backwashed with the chlorosilane liquid produced after supercharged exported using scrubbing tower circulating pump.
8. according to the processing unit described in any one of claim 1-4, which is characterized in that the dust removing units include the second pressure Poor table, the second control unit and two dedusters, two dedusters are connected in parallel, and one opens standby, second pressure difference Table is connect with the entrance and exit of two dedusters respectively, the front and back pressure difference for measuring deduster in operating status, institute The second control unit is stated to be used to cut off deduster in operating status when the measured value of the second differential pressure indicator is more than 0.1MPa, The deduster in stand-by state is switched to operating status simultaneously.
9. according to the processing unit described in any one of claim 1-4, which is characterized in that the multistage cooling unit includes sky Gas Cooler and freon cooler, the aerial cooler use eight, for carrying out cooling place to the fixed gas after dedusting Reason, most of chlorosilane condensate in the fixed gas after dedusting is got off and is sent to chlorosilane condensate liquid collecting tank, is exported simultaneously Remaining fixed gas is to freon cooler；The freon cooler is used to carry out cooling treatment to the remaining fixed gas, will Remaining chlorosilane condensate in the residue fixed gas gets off and is sent to chlorosilane condensate liquid collecting tank, while output contains impurity Hydrogen.
10. processing unit according to claim 9, which is characterized in that the multistage cooling unit further includes being located at air Cold and hot media heat exchanger between cooler and freon cooler is used to contain impurity using what freon cooler exported The cold of hydrogen carries out cooling treatment to the remaining fixed gas that aerial cooler exports, and will be condensed out during cooling treatment Chlorosilane be sent to chlorosilane condensate liquid collecting tank.
11. according to the processing unit described in any one of claim 1-4, which is characterized in that the processing unit further includes One delivery pump, for spraying the two level through scrubbing tower top after the chlorosilane condensate liquid supercharging in chlorosilane condensate liquid collecting tank Elution work is participated in inside mouth feeding scrubbing tower.
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CN111661827A (en) * 2020-06-22 2020-09-15 四川永祥多晶硅有限公司 System and method for recycling silicon powder in polycrystalline silicon reduction tail gas
CN112944205A (en) * 2021-03-12 2021-06-11 中国恩菲工程技术有限公司 Chlorosilane filling system and chlorosilane filling method
CN113426245A (en) * 2021-07-05 2021-09-24 四川炳辉环保科技有限责任公司 High-purity gas preparation method based on pressure swing adsorption
CN115804992A (en) * 2023-02-10 2023-03-17 山东东岳有机硅材料股份有限公司 Device and process for purifying methyl chlorosilane synthesis gas

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CN113426245B (en) * 2021-07-05 2022-11-22 四川炳辉环保科技有限责任公司 High-purity gas preparation method based on pressure swing adsorption
CN115804992A (en) * 2023-02-10 2023-03-17 山东东岳有机硅材料股份有限公司 Device and process for purifying methyl chlorosilane synthesis gas

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