CN102167331A - Collecting cooler for treating silicon tetrachloride (byproduct of polycrystalline silicon) - Google Patents

Collecting cooler for treating silicon tetrachloride (byproduct of polycrystalline silicon) Download PDF

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Publication number
CN102167331A
CN102167331A CN2011100665800A CN201110066580A CN102167331A CN 102167331 A CN102167331 A CN 102167331A CN 2011100665800 A CN2011100665800 A CN 2011100665800A CN 201110066580 A CN201110066580 A CN 201110066580A CN 102167331 A CN102167331 A CN 102167331A
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China
Prior art keywords
water cooler
inner casing
silicon tetrachloride
silicon
shell
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CN2011100665800A
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Chinese (zh)
Inventor
严大洲
毋克力
肖荣晖
汤传斌
谢正和
杜俊平
谢冬晖
汪绍芬
郭富东
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China ENFI Engineering Corp
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China ENFI Engineering Corp
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Priority to CN2011100665800A priority Critical patent/CN102167331A/en
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Abstract

The invention provides a collecting cooler for treating silicon tetrachloride (a byproduct of polycrystalline silicon), and the collecting cooler comprises an inner shell, an outer shell and a rotary body, wherein an inner cavity is limited in the inner shell; the upper part of the inner shell is provided with a feeding hole of the cooler, and the lower part of the inner shell is provided with a discharge hole of the cooler; the outer shell is sheathed outside the inner shell; a cooling medium space is limited by the inner shell and the outer shell; the lower part of the outer shell is provided with a cooling medium inlet, and the upper part of the outer shell is provided with a cooling medium outlet; and the rotary body is arranged in the cooling medium space along the vertical direction. When the collecting cooler provided by the embodiment of the invention is used for producing silicon dioxide by utilizing the silicon tetrachloride (the byproduct of polycrystalline silicon), hydrogen chloride and nanoscale silicon dioxide which are generated in the reaction of silicon tetrachloride, oxygen and hydrogen can be cooled in the collecting cooler; and the collecting cooler is simple in structure, low in cost and good in collecting and cooling effect.

Description

Be used for the collection water cooler that silicon tetrachloride as by-product of polysilicon is handled
Technical field
The present invention relates to a kind of collection water cooler, especially relate to a kind of collection water cooler that silicon tetrachloride as by-product of polysilicon is handled that is used for.
Background technology
In recent years, along with the development of silicon solar cell, polysilicon market is able to rapid growth.The polysilicon preparation method who adopts in the world is the Siemens Method of improvement at present, promptly adopt the trichlorosilane hydro-reduction, its by product mainly is a silicon tetrachloride, produce 1 ton of silicon tetrachloride as by-product that polysilicon produced and be approximately 12~18 tons, therefore how to handle the big bottleneck that silicon tetrachloride as by-product has become the polysilicon industrial development.
Summary of the invention
One object of the present invention is to propose a kind of collection water cooler that silicon tetrachloride as by-product of polysilicon is handled that is used for, this collection water cooler is used in silicon tetrachloride as by-product of polysilicon and produces in the silicon-dioxide, hydrogenchloride that silicon tetrachloride, oxygen and hydrogen reaction generate and nanometer grade silica are collected the water cooler internal cooling at this, and it is simple to collect cooler construction, cost is low, collects good cooling results.
The collection water cooler that is used for the silicon tetrachloride as by-product of polysilicon processing according to the embodiment of the invention comprises: inner casing, and described inner casing is limited with inner chamber, and the bottom that the top of described inner casing is provided with water cooler opening for feed and described inner casing is provided with the water cooler discharge port; Shell, described shell are set in described inner casing outside and limit the heat-eliminating medium space with described inner casing, and the top that the bottom of described shell is provided with heat-eliminating medium inlet and described shell is provided with the heat-eliminating medium outlet; With revolve body, the described body that revolves is arranged in the described heat-eliminating medium space along the vertical direction.
Collection water cooler according to the embodiment of the invention, be used in silicon tetrachloride as by-product of polysilicon and produce in the silicon-dioxide, hydrogenchloride that silicon tetrachloride, oxygen and hydrogen reaction generate and nanometer grade silica are collected the water cooler internal cooling at this, and it is simple to collect cooler construction, cost is low, collects good cooling results.
In addition, collection water cooler according to the above embodiment of the present invention can also have following additional technical characterictic:
The radial dimension edge direction from the top down that described inner casing and described shell are taper and described inner casing and described shell reduces gradually.
Described inner casing and described shell are taper shape.
Described water cooler opening for feed is formed on the top of described inner casing, and described water cooler discharge port is formed on the bottom of described inner casing.
Described heat-eliminating medium inlet is formed on the side of described shell and the upper end of contiguous described shell, and described heat-eliminating medium outlet is formed on the side of described shell and the lower end of contiguous described shell.
The described body that revolves comprises: a plurality of support bars, and described a plurality of support bars are along circumferential spaced apart setting; And rotating plate, described rotating plate links to each other with described a plurality of support bars and extends spirally along the vertical direction.
The described body that revolves further comprises ring flange, and the upper end of described a plurality of support bars links to each other with described ring flange respectively.
Additional aspect of the present invention and advantage part in the following description provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage are from obviously and easily understanding becoming the description of embodiment in conjunction with following accompanying drawing, wherein:
Fig. 1 is the block diagram that has according to the silicon tetrachloride as by-product of polysilicon treatment facility of the collection water cooler of the embodiment of the invention;
Fig. 2 is the synoptic diagram of the reactor of above-mentioned silicon tetrachloride as by-product of polysilicon treatment facility;
Fig. 3 is the synoptic diagram of the sparger of reactor shown in Figure 2;
Fig. 4 is the partial schematic diagram of sparger shown in Figure 3, wherein shows the arrangement mode of blade;
Fig. 5 is the synoptic diagram according to the collection water cooler of the embodiment of the invention;
Fig. 6 is the synoptic diagram of the inner casing of collection water cooler shown in Figure 5;
Fig. 7 is the synoptic diagram that revolves body of collection water cooler shown in Figure 5;
Fig. 8 is the synoptic diagram of the shell of collection water cooler shown in Figure 5;
Fig. 9 is the synoptic diagram of the collector of above-mentioned silicon tetrachloride as by-product of polysilicon treatment facility;
Figure 10 is the schematic top plan view of collector shown in Figure 9;
Figure 11 is the synoptic diagram of the gathering pipe of collector shown in Figure 9;
Figure 12 is the synoptic diagram of the depickling device of above-mentioned silicon tetrachloride as by-product of polysilicon treatment facility;
Figure 13 is the synoptic diagram of the expanding reach of depickling device shown in Figure 12;
Figure 14 is the synoptic diagram of the shaft of depickling device shown in Figure 12; With
Figure 15 is the operational flowchart of above-mentioned silicon tetrachloride as by-product of polysilicon treatment facility.
Embodiment
Describe embodiments of the invention below in detail, the example of described embodiment is shown in the drawings, and wherein identical from start to finish or similar label is represented identical or similar elements or the element with identical or similar functions.Below by the embodiment that is described with reference to the drawings is exemplary, only is used to explain the present invention, and can not be interpreted as limitation of the present invention.
In description of the invention, it will be appreciated that, term " " center "; " vertically "; " laterally "; " on "; D score; " preceding ", " back ", " left side ", " right side ", " vertically ", " level ", " top ", " end " " interior ", close the orientation of indications such as " outward " or position is based on orientation shown in the drawings or position relation, only be that the present invention for convenience of description and simplification are described, rather than the device or the element of indication or hint indication must have specific orientation, therefore orientation structure and operation with specific can not be interpreted as limitation of the present invention.
In description of the invention, need to prove that unless clear and definite regulation and qualification are arranged in addition, term " installation ", " linking to each other ", " connection " should be done broad understanding, for example, can be fixedly connected, also can be to removably connect, or connect integratedly; Can be directly to link to each other, also can link to each other indirectly by intermediary, can be the connection of two element internals.For the ordinary skill in the art, can particular case understand above-mentioned term concrete implication in the present invention.In addition, in an embodiment of the present invention, broad understanding should be made in term " mouth ", for example can be opening, also can be for being connected the form of one section pipe on the opening.
The present invention is based on the present inventor makes for solving a large amount of by products-silicon tetrachloride problem that produces in the production of polysilicon, a large amount of by product-the silicon tetrachloride of output in the production of polysilicon, produce one ton of polysilicon, according to different technology, meeting output 12-18 ton silicon tetrachloride, traditionally, silicon tetrachloride can't be handled proper application, has seriously restricted the development of production of polysilicon.The present invention adopts silicon tetrachloride as by-product of polysilicon to produce silicon-dioxide, has not only solved the outlet of the silicon tetrachloride as by-product of restriction production of polysilicon, recycle silicon tetrachloride as by-product of polysilicon.And the silicon-dioxide of production has purposes widely as typical nano-powder material, and for example car industry, construction industry and power industry mainly are the reinforced fillings as HTV and RTV silicon rubber; Also can be little with the shared production rolling resistance of carbon black, the tire anti-wet and slippery, that over-all properties is superior.This external other field industry also has a large amount of application, and the global demand total amount is near 150,000 tons/year at present, and annual growth is about 5%.Silicon-dioxide is at present in the usage quantity maximum of organosilicon industry, account for the over half of total consumption, all be widely used in this external rubber, plastics, high-performance coating and paint, printing ink, agricultural, chemically machinery polished, medicine and makeup, the papermaking, the market requirement and development potentiality are huge.Thus,, produce silicon-dioxide, not only promoted the development of production of polysilicon, and the silicon-dioxide of producing has purposes widely, realized efficiency of cycling economy with silicon tetrachloride as by-product of polysilicon according to the present invention.
In order to understand the collection water cooler that silicon tetrachloride as by-product of polysilicon is handled that is used for better, the silicon tetrachloride as by-product of polysilicon treatment facility that has according to the collection water cooler of the embodiment of the invention is described with reference to the drawings at first below according to the embodiment of the invention.
As shown in Figure 1, the silicon tetrachloride as by-product of polysilicon treatment facility that has according to the collection water cooler of the embodiment of the invention comprises the reactor 100 that connects successively, collects water cooler 200, collector 300, separator 400 and depickling device 500.
Silicon tetrachloride as by-product of polysilicon and air and hydrogen high-temperature combustion hydrolytic in reactor generates nano level silicon-dioxide.Silicon-dioxide enters from reactor 100 and collects water cooler 200 internal cooling, cooled silicon-dioxide enters collector 300 from collection water cooler 200 and is gathered into micron-sized silicon-dioxide, micron-sized silicon-dioxide after the gathering enters separator 400 and carries out gas solid separation, the solid that obtains (silicon-dioxide) enters 500 depicklings of depickling device, and the silicon-dioxide packing after the depickling is as product.
Preferably, the silicon tetrachloride as by-product of polysilicon treatment facility also comprises acid making system 600, and acid making system 600 links to each other with separator 400, be used for with hydrogenchloride relieving haperacidity after silicon-dioxide separates, thereby reduced pollution, increased efficiency of cycling economy.
The reactor 100 of silicon tetrachloride as by-product of polysilicon treatment facility is described below with reference to Fig. 2-4.
Shown in Fig. 2-4, according to embodiments of the invention, reactor 100 comprises reactor body 101, muzzle 104, annular space hydrogen inlet pipe 102 and sparger 102.
Be limited with reaction chamber in the reactor body 101, the top of reactor body 101 is provided with silicon tetrachloride-gas inlet 1012 and hydrogen inlet 1011, and the bottom of reactor body 101 is provided with reactor outlet 1013.
In example shown in Figure 2, reactor body 101 is the elongated cylindrical shell that extends along the vertical direction, hydrogen inlet 1011 is formed on the top of reactor body 101, the form of one section pipe that hydrogen inlet 1011 is communicated with the top of reactor body 101, and the center of departing from reactor body 101.The bottom end opening of reactor body 101 is to constitute reactor outlet 1013, and silicon tetrachloride-gas inlet 1012 is formed on the side (being the form of one section pipe among Fig. 2) on reactor body 101 tops.
Silicon tetrachloride as by-product of polysilicon and AIR MIXTURES enter reaction chamber from silicon tetrachloride-gas inlet 1012, and hydrogen enters reactor from hydrogen inlet 1011.
The lower end that muzzle 104 is set in reactor body 101 is to limit annular space H to lower opening with reactor body 101.For example, the upper end of muzzle 104 is enclosed within on the reactor body 101 and by bolt and holds out against.
Annular space hydrogen inlet pipe 103 links to each other with hydrogen supply in annular space H with muzzle 104, lights a fire thus, and combustion reactions takes place in the lower end of reactor body 101, because annular space H, makes the temperature-stable of flame kernel.
Sparger 102 is arranged in the reaction chamber, be used for uniform distribution and supply to silicon tetrachloride-air and hydrogen in the reaction chamber from silicon tetrachloride-gas inlet 1012 and hydrogen inlet 1011, avoid air-flow directly to dash downwards, make the combustion reactions better effects if from the top of reaction chamber.
According to embodiments of the invention, reactor 100 simple in structure, easy to operate, the reaction effect of silicon tetrachloride, air and hydrogen is good.
As shown in Figure 2, in a specific embodiment of the present invention, reactor body 101 is for elongated cylindrical shell and comprise mouth body 1014, mouth body 1015 and sharp-tongued 1016.As shown in Figure 2, in concrete examples more of the present invention, mouth body 1014, mouth body 1015 and sharp-tongued 1016 also is respectively round shape and their internal diameter reduces successively.
Silicon tetrachloride-gas inlet 1012 is arranged on the side of mouth body 1014 and the top that hydrogen inlet 1011 is arranged on mouth body 1014.Particularly, the top and bottom of mouth body 1014 are opened wide, and the upper end can seal with top cover, and hydrogen inlet 1011 runs through top cover and forms, and connects one section pipe (also can be called the hydrogen inlet pipe) at hydrogen inlet 1011 places.
The upper end of mouth body 1015 links to each other with the lower end of mouth body 1014, for example mouth body 1015 is threaded with mouth body 1014, as shown in Figure 2, the upper end of mouth body 1015 is provided with outside screw, the lower end of mouth body 1014 is provided with internal thread, and on mouth body 1015, be combined with mouth mother 1017, so that in the space that mouth female 1017 and mouth body 1015 and mouth body 1014 limit, filler 1018 is set.
Sharp-tongued 1016 upper end links to each other with the lower end of mouth body 1015, for example, and also by being threaded.Sharp-tongued 1016 lower end is opened wide to form reactor outlet 1013.As shown in Figure 2, it is concordant with sharp-tongued 1016 lower end that muzzle 104 is installed in the lower end of described sharp-tongued lower end and muzzle 104.The bottom of muzzle 104 is taper, thereby the radial dimension of annular space H reduces downwards gradually.
As Fig. 2-shown in Figure 4, sparger 102 comprises strut 1021 and a plurality of blade 1022.One end of each blade 1022 links to each other with strut 1021 and a plurality of blade 1022 circumferentially spaced apart along strut 1021.
As shown in Figure 3, in some embodiments of the invention, a plurality of blades were organized 1022 minutes more, and the blade 1022 in every group is along the circumferential arranged spaced apart of strut 1021 and to organize blade 1022 spaced apart along the vertical direction more.Preferably, be positioned at the upper end of nethermost one group of blade 1022 contiguous muzzle 104 on above-below direction.
In the example depicted in fig. 3, blade 1022 is divided into three groups, is positioned at the upper end of uppermost one group of blade 1022 contiguous sharp-tongued 1016, is positioned at the upper end of nethermost one group of blade, 1022 contiguous muzzles 104.Be understandable that the present invention is not limited to this, blade 1022 can be divided into the group of any suitable quantity.
As mentioned above, sparger 102 be used to distribute enter into reactor 100 reaction chamber in silicon tetrachloride and the air-flow of air and hydrogen, avoid air-flow directly directly to rush at the bottom, thereby improve the specific surface area that combustion conditions is controlled silicon-dioxide from reaction chamber top.
According to reactor 100 of the present invention, silicon tetrachloride and AIR MIXTURES enter reaction chamber from silicon tetrachloride-gas inlet 1012, and hydrogen enters reaction chamber from hydrogen inlet 1011, flow downward after distributing by divider 102 then.In addition, hydrogen supplies in the annular space H from annular space hydrogen inlet pipe 103, in the lower end (more specifically, at sharp-tongued 1016 places) of reactor 100 combustion reactions takes place, and produces the silicon-dioxide of hydrogen chloride gas and nano level (for example 7-40 nanometer).Need to prove that temperature is approximately 1700 degrees centigrade in the reactor 100, the air pressure in the reaction chamber is lower than normal atmosphere, for example negative 1.84 kPas.
Below with reference to be used for the collection water cooler 200 that silicon tetrachloride as by-product of polysilicon handle of Fig. 5-8 description according to the embodiment of the invention.
Collection water cooler 200 according to the embodiment of the invention links to each other with reactor 100, is used to cool off hydrogen chloride gas and the nano level silicon-dioxide that generates in the reaction of reactor 100 internal combustion.For example, collect the below that water cooler 200 can be located at reactor 100, hydrogen chloride gas that reactor 100 internal reactions generate and nano level silicon-dioxide enter to collect in the water cooler 200 and cool off.
Shown in Fig. 5-8, according to embodiments of the invention, collect water cooler 200 and comprise inner casing 201, shell 203 and revolve body 202.
Inner casing 201 is limited with inner chamber, and the top of inner casing 201 is provided with water cooler opening for feed 2011, and the bottom of inner casing 201 is provided with water cooler discharge port 2012.Preferably, water cooler opening for feed 2011 is formed on the top of inner casing 201, and water cooler discharge port 2012 is formed on the bottom of inner casing 201, and in other words, the top and bottom of inner casing 201 are opened wide to constitute water cooler opening for feed 2011 and water cooler discharge port 2012 respectively.
As mentioned above, reactor 100 is located at the top of collecting water cooler 200, and reactor outlet 1013 is relative with water cooler opening for feed 2011, for example at a distance of 3-5 centimetre.Flow from the top down in high-temp chlorination hydrogen that comes out from reactor outlet 1013 and silicon-dioxide enter inner casing 201 from water cooler opening for feed 2011 the inner chamber.
Shell 203 is set in inner casing 201 outsides to limit the heat-eliminating medium space with inner casing 201, and the bottom of shell 203 is provided with heat-eliminating medium inlet 2031, and the top of shell 203 is provided with heat-eliminating medium outlet 2032.Heat-eliminating medium for example is an air, air enters in the heat-eliminating medium space from heat-eliminating medium inlet 2031, flow from bottom to top, and finally discharge the heat-eliminating medium spaces from heat-eliminating medium outlet 2032, thus cooling mobile hydrogenchloride and silicon-dioxide from the top down in the inner chamber of inner casing 201.
Preferably, heat-eliminating medium inlet 2031 is formed on the side of shell 203 and the upper end of adjacent housings 203, and heat-eliminating medium outlet 2032 is formed on the side of shell 203 and the lower end of adjacent housings 203.
Revolve body 202 and be arranged on along the vertical direction in the heat-eliminating medium space, revolve body 202 and be used for cooling air is evenly distributed in the heat-eliminating medium space, so that improve the cooling performance of mobile hydrogenchloride and silicon-dioxide from the top down in the inner chamber of inner casing 201.
The pressure of collecting in the water cooler 200 also is lower than normal atmosphere, and hydrogenchloride and silicon-dioxide are cooled off about 500-800 degree centigrade, so that subsequent disposal.
Shown in Fig. 5-8, in some embodiments of the invention, inner casing 201 and shell 203 are taper, and more specifically, inner casing 201 and shell 203 are taper shape, and the radial dimension of inner casing 201 and shell 203 reduces gradually along direction from the top down.
As Fig. 5 and shown in Figure 7, revolve body 202 and comprise a plurality of support bars 2021 and rotating plate 2022, a plurality of support bars 2021 are along circumferential spaced apart setting, and rotating plate 2022 links to each other with a plurality of support bars 2021 and extends spirally along the vertical direction.As mentioned above, the rotating plate 2022 that revolves in the body 202 is used for cooling air is distributed in the whole cooling space, thereby improves cooling performance.Similar with the shape of inner casing 201 and shell 203, for example form up big and down small taper shape.
As shown in Figure 7, revolve body 202 and further comprise ring flange 2023, the upper end of a plurality of support bars 2021 links to each other with ring flange 2023 respectively, revolve body 202 and can be installed to the upper end of inner casing 201 by ring flange 2023, upper end at inner casing 201 also is formed with corresponding flange, ring flange 2023 is placed on the described flange, and connects with bolt.
According to embodiments of the invention, collect the simple in structure of water cooler 200, to the good cooling results of hydrogenchloride and silicon-dioxide.
The collector 300 of above-mentioned silicon tetrachloride as by-product of polysilicon treatment facility is described below with reference to Fig. 9-11.
According to embodiments of the invention, collector 300 links to each other with collection water cooler 200, be used to make cooled silicon-dioxide to assemble therein, thereby nano level silica aggregate becomes the silicon-dioxide of micron order (for example 30-50 micron), use so that can be used as finished product.
Shown in Fig. 9-11, according to embodiments of the invention, collector 300 comprises a plurality of gathering pipes 301, the accumulation chamber that a plurality of gathering pipes 301 link to each other and extend with curve form to limit successively, first in wherein a plurality of gathering pipes 301 are assembled the free end of pipe (nethermost gathering pipe among Fig. 9) and are assembled the free end of pipe (the uppermost gathering pipe among Fig. 9) as collector outlet 3012 as collector inlet 3011 and last.
In other words, a plurality of gathering pipes 301 join end to end successively and extend in the zigzag mode.
Collector inlet 3011 links to each other with the water cooler discharge port 2012 of collecting cooling 200, thereby cooled hydrogenchloride and nanometer grade silica of discharging from water cooler discharge port 2012 enters in the accumulation chamber from collector inlet 3011, when in the accumulation chamber that tortuous mode is extended, advancing, in Fig. 9, advance silicon-dioxide and the inwall of assembling pipe 301 and collide each other and be gathered into micron-sized silicon-dioxide from bottom to top.
According to embodiments of the invention, collector 300 simple in structure, easily manufactured, congregational rate is good.
In some embodiments of the invention, a plurality of gathering pipes 301 are connected to each other to a plurality of zigzags, thereby the accumulation chamber of described curve form is made of a plurality of zigzags.As shown in Figure 9, two adjacent gathering pipes 301 stagger on the direction (above-below direction among Fig. 9) that described accumulation chamber is extended each other.
Preferably, shown in Figure 10 and 11, each assembles two elbow sections that pipe 301 comprises straight-line segment and is positioned at the straight-line segment two ends, free end in described two elbow sections is respectively equipped with joint flange 302, adjacent gathering pipe 301 links to each other by joint flange 302, links to each other thereby be convenient to a plurality of gathering pipes 301.
As shown in figure 10, preferably, be respectively equipped with gauge hatch 303 on first gathering pipe and last gathering pipe, be respectively equipped with the detector (not shown) that is used to detect the temperature and pressure in the described accumulation chamber in the gauge hatch 303.
According to embodiments of the invention, the pressure in the collector 300 also can be less than normal atmosphere, and the temperature of the silicon-dioxide after the gathering is approximately 150 degrees centigrade.
According to the embodiment of the invention, collector 300 can be used for nano level silica aggregate is become micron-sized silicon-dioxide, and simple in structure, and cost is low.
Below the simple separator 400 of describing above-mentioned silicon tetrachloride as by-product of polysilicon treatment facility.Separator 400 is used for hydrogenchloride is separated with micron-sized silicon-dioxide, and separator 400 can be used any suitable gas-solid separator in this area.Separator 400 has separator inlet, pneumatic outlet and solid outlet, wherein said separator inlet links to each other with collector outlet 3012, thereby the silicon-dioxide after assembling and hydrogenchloride enter separator 400 so that hydrogenchloride is separated with silicon-dioxide from collector outlet 3012 by separator inlet, hydrogenchloride is discharged from pneumatic outlet, for example deliver to acid making system 600 and carry out relieving haperacidity, thereby reduced pollution, improved efficiency of cycling economy.
Preferably, separator 400 is a three-stage cyclone separator, and three-stage cyclone separator is connected successively, thereby improves the separating effect of hydrogenchloride and silicon-dioxide.And then separator 400 can also comprise the deep bed filter that links to each other with the last step cyclonic separator, with further raising separating effect.
The depickling device 500 of above-mentioned silicon tetrachloride as by-product of polysilicon treatment facility is described below with reference to Figure 12-14.
From the surface of separator 400 isolated silicon-dioxide, can be attached with hydrogenchloride, therefore, deliver to depickling device 500 from separator 400 isolated silicon-dioxide and carry out depickling to remove the hydrogenchloride that silica sphere adheres to, the silicon-dioxide that obtains thus can be packed as finished product.
Shown in Figure 12-14, according to embodiments of the invention, depickling device 500 comprises depickling device body and heating tube 503.
Be limited with the depickling chamber in the depickling device body, described depickling device upper part of body is provided with tail gas outlet 5014 and depickling device discharge port 5013, and the bottom of described depickling device body is provided with depickling steam-in 5011 and depickling device opening for feed 5012.Heating tube 503, quartz electric heating pipe for example is arranged on the described depickling device body and stretches in the described depickling chamber.
Depickling device opening for feed 5012 links to each other with the solid outlet of separator 400, thereby enters in the depickling chamber from depickling device opening for feed 5012 with silicon-dioxide after hydrogenchloride separates.Depickling steam enters the depickling chamber from depickling steam-in 5011, in the depickling chamber, move along direction from bottom to top with silicon-dioxide, in the process that moves upward, depickling steam is sloughed the hydrogenchloride that silica sphere adheres to, and in uphill process, 503 pairs of depickling steam of heating tube and silicon-dioxide heating, thus deacidification effect improved.
Silicon-dioxide after the depickling is discharged from depickling device discharge port 5013, and the tail gas after the depickling is discharged from tail gas outlet 5014, and tail gas outlet 5014 can link to each other with acid making system 600, and the hydrogenchloride of sloughing from silica sphere can be used for relieving haperacidity.Alternatively, tail gas outlet 5014 also can link to each other with the separator inlet of separator 400, and the silicon-dioxide that is used for tail gas is carried secretly separates with hydrogenchloride, and the silicon-dioxide after the separation enters the hydrogenchloride that depickling device 500 is sloughed surface attachment.
According to embodiments of the invention, the pressure in the depickling device 500 also can be lower than normal atmosphere, for example negative 2.1 kPas.
Shown in Figure 12-14, in specific embodiments more of the present invention, described depickling device body comprises expanding reach 501, shaft 502 and furnace bottom 503.For example, expanding reach 501, shaft 502 and furnace bottom 503 can be solid of revolution, and their internal diameter reduces successively.
The bottom of expanding reach 501 is a truncated cone shape, frustoconical for example, and the top of expanding reach 501 is round shape.Tail gas outlet 5014 top and the depickling device discharge ports 5013 that are formed on expanding reach 501 are formed on the inclined-plane of expanding reach 501 bottoms.
Shown in Figure 12 and 13, in some embodiments of the invention, the side of expanding reach 501 is provided with material level and detects mouth 5017, and material level detects mouth 5017 and is higher than depickling device discharge port 5013, is used to detect the material level in the expanding reach 501.Alternatively, also be provided with porthole 5016 on the side of expanding reach 501, impenetrating mouth 5016 can be relative with material level detection mouth 5017.
As described in Figure 12 and 13, in a preferred embodiment of the invention, the side of expanding reach 501 is provided with balance port 5015, and balance port 5015 is used for the pressure in the balance depickling chamber, and for example, balance port 5015 can link to each other with the separator inlet of separator 400.
Shaft 502 can round shape, and the upper end of shaft 502 links to each other with the lower end of expanding reach 501, and wherein heating tube 503 is installed on the shaft 502.Shown in Figure 12 and 14, heating tube 503 can be distributed on the whole surface of shaft 502.The internal diameter of shaft 502 is less than the internal diameter on expanding reach 501 tops, and for easy to connect, the external diameter of shaft 502 and internal diameter are can be respectively identical with the external diameter and the internal diameter of the lower end of expanding reach 501.
As Figure 12 and shown in Figure 14, in a preferred embodiment of the invention, be respectively equipped with on the side of shaft 502 and purge mouth 5018 and temperature-measuring port, purge mouthful top and bottom that are respectively adjacent to shaft 502, purge mouth 5018 and be used for shaft 502 inner chambers are purged, avoid silicon-dioxide in shaft 502, to accumulate.Be provided with temperature element 504 in the temperature-measuring port, be used to measure the temperature in the shaft 502.
The upper end of furnace bottom 503 links to each other with shaft 502 and depickling steam-in 5011 and depickling device opening for feed 5012 are respectively formed on the side of furnace bottom 503.As shown in figure 12, furnace bottom 503 tops are cylindrical section, and the bottom of furnace bottom 503 is a conical section, and for easy to connect, the external diameter of the cylindrical section of furnace bottom 503 and internal diameter external diameter and the internal diameter with the lower end of shaft 502 respectively are identical.
As shown in figure 12, the bottom of furnace bottom 503 is provided with slag-drip opening 5019, is used to discharge bigger silica dioxide granule.
According to embodiments of the invention, enter in the depickling chamber from depickling device opening for feed 5012 with the isolating micron-sized silicon-dioxide of hydrogen chloride gas, steam enters in the depickling chamber from depickling steam-in 5011, silicon-dioxide and steam is motion from bottom to top in the depickling chamber, in the process of motion, steam is sloughed the hydrogenchloride that silica sphere adheres to, and sloughs the silicon-dioxide of the hydrogenchloride of surface attachment and discharges from depickling device discharge port 5013, packs as finished product.
Steam and the hydrogenchloride of sloughing from silica sphere are discharged from tail gas outlet 5014, can deliver to acid making system 600 relieving haperacidity, also can deliver in the separator 400 to isolate the silicon-dioxide of carrying secretly in the tail gas.In this process, balance port 5015 can link to each other with separator 400, with the pressure in the balance depickling chamber, and separates with the silicon-dioxide of wherein carrying secretly in separator 400 from the steam that balance port 5015 is come out.
According to embodiments of the invention, the silicon tetrachloride as by-product of polysilicon treatment facility can be handled silicon tetrachloride as by-product of polysilicon, the micron silica that production serves many purposes, the problem of the restriction production of polysilicon of Xie Jueing not only, and improved efficiency of cycling economy.In addition, according to embodiments of the invention, treating processes can be carried out under the negative pressure, flows between each integral part of treatment facility and conveying thereby be convenient to material.
The treatment scheme of silicon tetrachloride as by-product of polysilicon is described below with reference to Figure 15.
At first, supply with silicon tetrachloride, hydrogen and oxygen-containing gas in reactor 100, silicon tetrachloride mixes with hydrogen and supplies in the reactor 100, and oxygen-containing gas for example is an air.The high-temperature combustion hydrolytic reaction takes place in silicon tetrachloride, hydrogen and oxygen in reactor 100, comprise first gas-solid mixture of hydrogen chloride gas and nanometer grade silica with generation.
Particularly, the temperature in the reactor 100 may be controlled to about 1700 degrees centigrade, and pressure may be controlled to than atmosphere and forces down 1.8 kPas.The granularity of silicon-dioxide for example is the 7-40 nanometer.
Next, it is interior to cool off described first gas-solid mixture that first gas-solid mixture is introduced collection water cooler 200, for example first gas-solid mixture is cooled to about 500-800 degree centigrade.
Cooled described first gas-solid mixture is introduced in the collector 300, and described nanometer grade silica is assembled by collision in collector 300, obtains comprising second gas-solid mixture of hydrogen chloride gas and micron silica.For example, the granularity of micron-sized silicon-dioxide is the 30-50 micron.
To separate in described second gas-solid mixture introducing separator 400, obtain micron silica and first tail gas that contains hydrogenchloride.As mentioned above, separator 400 can be cyclonic separator, and for example, described second gas-solid mixture can carry out first tail gas that three grades of cyclonic separation obtain described micron silica and contain hydrogen chloride gas.Alternatively, first tail gas after three grades of cyclonic separation can separate by the cloth bag type separator more once more.
At last, described micron-sized silicon-dioxide is introduced in the depickling device 500, removed the hydrogenchloride of described micron silica surface attachment, obtain silicon-dioxide finished product and second tail gas that contains hydrogen chloride gas to propose the depickling processing by steam gas.The specific surface area of described silicon-dioxide finished product can be about 150-380m 2Outside can packing ,/g, silicon-dioxide finished product sell.
In some embodiments of the invention, described first tail gas and second tail gas can be delivered to acid making system and be prepared hydrochloric acid, and alternatively, described second tail gas can be back to separator 400 and carry out secondary separation.
Preferably, reactor 100, collection water cooler 200, collector 300, cyclonic separator 400, the pressure in the depickling device 500 all are lower than normal atmosphere, in other words, combustion reactions, cooling, assemble, separation and depickling are all carried out under negative pressure, thereby help the conveying of material in the rising container.
According to embodiments of the invention, can produce micron silica (also can be called aerosil) with silicon tetrachloride as by-product of polysilicon, micron silica has purposes widely, tail gas can be used for relieving haperacidity, the restraining factors of restriction production of polysilicon have not only been solved, for silicon tetrachloride as by-product has found outlet, and the silicon-dioxide of producing is the product with extensive use, improved efficiency of cycling economy.
In the description of this specification sheets, concrete feature, structure, material or characteristics that the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means in conjunction with this embodiment or example description are contained at least one embodiment of the present invention or the example.In this manual, the schematic statement to above-mentioned term not necessarily refers to identical embodiment or example.And concrete feature, structure, material or the characteristics of description can be with the suitable manner combination in any one or more embodiment or example.
Although illustrated and described embodiments of the invention, those having ordinary skill in the art will appreciate that: can carry out multiple variation, modification, replacement and modification to these embodiment under the situation that does not break away from principle of the present invention and aim, scope of the present invention is limited by claim and equivalent thereof.

Claims (7)

1. one kind is used for the collection water cooler that silicon tetrachloride as by-product of polysilicon is handled, and it is characterized in that, comprising:
Inner casing, described inner casing is limited with inner chamber, and the bottom that the top of described inner casing is provided with water cooler opening for feed and described inner casing is provided with the water cooler discharge port;
Shell, described shell are set in described inner casing outside and limit the heat-eliminating medium space with described inner casing, and the top that the bottom of described shell is provided with heat-eliminating medium inlet and described shell is provided with the heat-eliminating medium outlet; With
Revolve body, the described body that revolves is arranged in the described heat-eliminating medium space along the vertical direction.
2. the collection water cooler that is used for the silicon tetrachloride as by-product of polysilicon processing according to claim 1 is characterized in that, the radial dimension edge direction from the top down that described inner casing and described shell are taper and described inner casing and described shell reduces gradually.
3. the collection water cooler that is used for the silicon tetrachloride as by-product of polysilicon processing according to claim 2 is characterized in that described inner casing and described shell are taper shape.
4. the collection water cooler that is used for the silicon tetrachloride as by-product of polysilicon processing according to claim 1 is characterized in that described water cooler opening for feed is formed on the top of described inner casing, and described water cooler discharge port is formed on the bottom of described inner casing.
5. the collection water cooler that is used for the silicon tetrachloride as by-product of polysilicon processing according to claim 4, it is characterized in that, described heat-eliminating medium inlet is formed on the side of described shell and the upper end of contiguous described shell, and described heat-eliminating medium outlet is formed on the side of described shell and the lower end of contiguous described shell.
6. according to each described collection water cooler that is used for the silicon tetrachloride as by-product of polysilicon processing among the claim 1-5, it is characterized in that the described body that revolves comprises:
A plurality of support bars, described a plurality of support bars are along circumferential spaced apart setting; With
Rotating plate, described rotating plate links to each other with described a plurality of support bars and extends spirally along the vertical direction.
7. the collection water cooler that is used for the silicon tetrachloride as by-product of polysilicon processing according to claim 6 is characterized in that the described body that revolves further comprises ring flange, and the upper end of described a plurality of support bars links to each other with described ring flange respectively.
CN2011100665800A 2011-03-18 2011-03-18 Collecting cooler for treating silicon tetrachloride (byproduct of polycrystalline silicon) Pending CN102167331A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113401912A (en) * 2021-07-06 2021-09-17 苏州大学 Device and method for regulating and controlling size of silica particles synthesized by flame method
CN115626648A (en) * 2022-12-02 2023-01-20 中国恩菲工程技术有限公司 Silicon tetrachloride cold hydrogenation system and silicon tetrachloride cold hydrogenation method

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CN2564972Y (en) * 2002-05-16 2003-08-06 陈家富 Spiral flow guiding cooler
CN201363739Y (en) * 2008-11-20 2009-12-16 无锡锡东能源科技有限公司 Water-cooled screw slag extractor
CN202054618U (en) * 2011-03-18 2011-11-30 中国恩菲工程技术有限公司 Collection cooler for treating silicon tetrachloride serving as polysilicon byproduct

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Publication number Priority date Publication date Assignee Title
CN2268241Y (en) * 1995-12-14 1997-11-19 杨柯 Drum type heat-exchanger
CN1399116A (en) * 2001-07-25 2003-02-26 化学工业第二设计院 Spiral-shell tubular heat exchanger
CN2564972Y (en) * 2002-05-16 2003-08-06 陈家富 Spiral flow guiding cooler
CN201363739Y (en) * 2008-11-20 2009-12-16 无锡锡东能源科技有限公司 Water-cooled screw slag extractor
CN202054618U (en) * 2011-03-18 2011-11-30 中国恩菲工程技术有限公司 Collection cooler for treating silicon tetrachloride serving as polysilicon byproduct

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113401912A (en) * 2021-07-06 2021-09-17 苏州大学 Device and method for regulating and controlling size of silica particles synthesized by flame method
CN113401912B (en) * 2021-07-06 2023-03-07 苏州大学 Device and method for regulating and controlling size of silica particles synthesized by flame method
CN115626648A (en) * 2022-12-02 2023-01-20 中国恩菲工程技术有限公司 Silicon tetrachloride cold hydrogenation system and silicon tetrachloride cold hydrogenation method
CN115626648B (en) * 2022-12-02 2023-03-28 中国恩菲工程技术有限公司 Silicon tetrachloride cold hydrogenation system and silicon tetrachloride cold hydrogenation method

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Application publication date: 20110831