CN102167333B - Equipment for processing silicon tetrachloride as byproduct of polysilicon - Google Patents
Equipment for processing silicon tetrachloride as byproduct of polysilicon Download PDFInfo
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- CN102167333B CN102167333B CN201110066588A CN201110066588A CN102167333B CN 102167333 B CN102167333 B CN 102167333B CN 201110066588 A CN201110066588 A CN 201110066588A CN 201110066588 A CN201110066588 A CN 201110066588A CN 102167333 B CN102167333 B CN 102167333B
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Abstract
The invention discloses equipment for processing silicon tetrachloride as a byproduct of polysilicon. The equipment comprises a reactor, a collecting cooler, a gathering device a separator and a deacidifying device, wherein the collecting cooler is arranged below the reactor so as to facilitate the connection between a feed port of the cooler and an outlet of the reactor; an inlet of the gathering device is connected with a discharge port of the cooler; the separator is provided with a separator inlet, a gas outlet and a solid outlet, and the separator inlet is connected with the outlet of the gathering device; and the upper part of the deacidifying device is provided with a tail gas outlet and a discharge port of the deacidifying device, the lower part of the deacidifying device is provided with a steam inlet and a feed port of the deacidifying device, and the feed port of the deacidifying device is connected with the solid outlet of the separator. According to the equipment for processing the silicon tetrachloride as the byproduct of the polysilicon in the invention, the silicon tetrachloride as the byproduct of the polysilicon can be used for producing micrometer-grade silicon diode, so that the problem that the silicon tetrachloride as the byproduct restricts the production of the polysilicon is solved, the produced micrometer-grade silicon dioxide has extensive applications, and a circular economy effect is enhanced; and in addition, the equipment has the advantages of simple structure, simplicity for operation and low cost.
Description
Technical field
The present invention relates to a kind of silicon tetrachloride as by-product of polysilicon treatment facility, especially relate to a kind of treatment facility of producing silicon-dioxide by silicon tetrachloride as by-product of polysilicon.
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 at present is the Siemens Method of improvement; 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 silicon tetrachloride as by-product of polysilicon treatment facility; Utilize this treatment facility can the recycle silicon tetrachloride as by-product of polysilicon; Both used silicon tetrachloride as by-product of polysilicon to produce silicon-dioxide; Improve efficiency of cycling economy, promoted the development of production of polysilicon.
Silicon tetrachloride as by-product of polysilicon treatment facility according to the embodiment of the invention; Comprise: reactor drum; In having, said reactor drum is limited with reaction chamber; The top of said reactor drum is provided with silicon tetrachloride-gas inlet and hydrogen inlet, and the bottom that the bottom of said reactor drum is provided with ring hydrogen inlet and said reactor drum is provided with reactor outlet; Collect water cooler; Be limited with inner chamber and the heat-eliminating medium space that is enclosed within the inner chamber outside and separates in the said collection water cooler with inner chamber; The top of said collection water cooler be provided with the water cooler opening for feed that is communicated with said inner chamber and with the heat-eliminating medium outlet of said heat-eliminating medium spatial communication; The bottom of said collection water cooler be provided with the water cooler discharge port that is communicated with said inner chamber and with the cooling medium inlet of said heat-eliminating medium spatial communication, wherein said collection water cooler is positioned at said reactor drum below so that said water cooler opening for feed links to each other with said reactor outlet; Collector, said collector have collector inlet and collector outlet, and wherein said collector inlet links to each other with said water cooler discharge port; Separator, said separator has separator inlet, pneumatic outlet and solid outlet, and wherein said separator inlet links to each other with said collector outlet; With the depickling device; In having, said depickling utensil is limited with the depickling chamber; The top of said depickling device is provided with tail gas outlet and depickling device discharge port, and the bottom of said depickling device is provided with steam-in and depickling device opening for feed, and wherein said depickling device opening for feed links to each other with the solid outlet of said separator.
Silicon tetrachloride as by-product of polysilicon treatment facility according to the embodiment of the invention; Can produce micron silica with silicon tetrachloride as by-product of polysilicon; Not only solved silicon tetrachloride as by-product restriction production of polysilicon, and the micron silica of producing has purposes widely, improved the recycling economy effect; And structure and simple to operate, cost is low.
In addition, can also have following additional technical characterictic according to the above embodiment of the present invention silicon tetrachloride as by-product of polysilicon treatment facility:
Silicon tetrachloride as by-product of polysilicon treatment facility according to the embodiment of the invention also comprises acid making system, and said acid making system links to each other with the pneumatic outlet of said separator.
The tail gas outlet of said depickling device links to each other with said separator inlet.
Said separator is a three-stage cyclone separator.
Said separator also comprises the deep bed filter that links to each other with the last step cyclonic separator.
Said reactor drum comprises: reactor body, said reaction chamber are limited in the said reactor body, and said silicon tetrachloride-gas inlet and hydrogen inlet are located at the top of said reactor body, and said reactor outlet is located at the bottom of said reactor body; Muzzle, said muzzle are set in the lower end of said reactor body to limit the annular space to lower opening with said reactor body; Annular space hydrogen inlet pipe, said annular space hydrogen inlet pipe link to each other with said muzzle with hydrogen supply in said annular space; And sparger, said sparger is arranged on and is used for uniform distribution in the said reaction chamber and supplies to silicon tetrachloride-air and hydrogen in the reaction chamber from said silicon tetrachloride-gas inlet and said hydrogen inlet.
Said reactor body comprises: mouth body, said silicon tetrachloride-gas inlet are arranged on the side of said mouth body and the top that said hydrogen inlet is arranged on said mouth body; The mouth body, the lower ends of the upper end of said mouth body and said mouth body; Sharp-tongued, the said sharp-tongued upper end and the lower ends of said mouth body, said sharp-tongued lower end is opened wide to form said reactor outlet.
Said collection water cooler comprises: inner casing, said inner chamber are limited in the said inner casing, and said water cooler opening for feed is located at the top of said inner casing and the bottom that said water cooler discharge port is located at said inner casing; Shell, said shell are set in said inner casing outside, and said heat-eliminating medium space boundary is between said inner casing and said shell, and said heat-eliminating medium inlet is located at the bottom of said shell and the top that the outlet of said heat-eliminating medium is located at said shell; With revolve body, the said body that revolves is arranged in the said heat-eliminating medium space along the vertical direction.
Said collector comprises: a plurality of gathering pipes; Said a plurality of gathering pipe is continuous successively to limit the accumulation chamber of extending with curve form, and first in wherein said a plurality of gathering pipes assembled the free end that free end enters the mouth as said collector and last assembles pipe of pipe as said collector outlet.
Said depickling device; Comprise: depickling device body; Said depickling chamber is limited in the said depickling device body, and said tail gas outlet and depickling device discharge port are located at said depickling device upper part of body, and said steam-in and depickling device opening for feed are located at the bottom of said depickling device body; And heating tube, said heating tube is arranged on the said depickling device body and stretches in the said depickling chamber.
Said depickling device body comprises: expanding reach, the bottom of said expanding reach are truncated cone shape, and top and said depickling device discharge port that said tail gas outlet is formed on said expanding reach are formed on the inclined-plane of said expanding reach bottom; Shaft, the upper end of said shaft and the lower ends of said expanding reach, wherein said heating tube is installed on the said shaft; And furnace bottom, the upper end of said furnace bottom links to each other with said shaft and said depickling steam-in and said depickling device opening for feed are respectively formed on the side of furnace bottom.
The bottom of said furnace bottom is provided with slag-drip opening, is respectively equipped with on the side of said shaft to purge mouth and temperature-measuring port, and the top and bottom of the contiguous said shaft of said purging mouth, the side of said expanding reach is provided with balance port.
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 through practice of the present invention.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage obviously with are easily understood becoming the description of embodiment from combining figs, wherein:
Fig. 1 is the block diagram according to the silicon tetrachloride as by-product of polysilicon treatment facility of the embodiment of the invention;
Fig. 2 is the synoptic diagram according to the reactor drum of the silicon tetrachloride as by-product of polysilicon treatment facility of the embodiment of the invention;
Fig. 3 is the synoptic diagram of the sparger of reactor drum 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 silicon tetrachloride as by-product of polysilicon treatment facility 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 according to the collector of the silicon tetrachloride as by-product of polysilicon treatment facility of the embodiment of the invention;
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 according to the depickling device of the silicon tetrachloride as by-product of polysilicon treatment facility of the embodiment of the invention;
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 according to the silicon tetrachloride as by-product of polysilicon treatment facility of the embodiment of the invention.
Embodiment
Describe embodiments of the invention below in detail, the example of said 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.Be exemplary through the embodiment that is described with reference to the drawings below, only be 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; The orientation of indications such as term " " center ", " vertically ", " laterally ", " on ", D score, " preceding ", " back ", " left side ", " right side ", " vertically ", " level ", " top ", " end " " interior ", " outward " or position relation are for based on orientation shown in the drawings or position relation; only be to describe with simplifying for the ease of describing the present invention; rather than the device or the element of indication or hint indication must have specific orientation, with specific azimuth configuration and operation, therefore can not be interpreted as limitation of the present invention.
In description of the invention, need to prove that only if 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 to 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 through intermediary, can be the connection of two element internals.For those of 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 is produced one ton of polysilicon, according to different processes; 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 sector mainly are the reinforced fillings as HTV and RTV Zylox; 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 number of applications, and the global demand total amount is near 150,000 tons/year at present, and annual growth is about 5%.Silicon-dioxide is maximum in the usage quantity of organosilicon industry at present; 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.
Silicon tetrachloride as by-product of polysilicon treatment facility according to the embodiment of the invention is described with reference to the drawings below.
As shown in Figure 1, comprise the reactor drum 100 that connects successively according to the silicon tetrachloride as by-product of polysilicon treatment facility of the embodiment of the invention, collect 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 drum generates nano level silicon-dioxide.Silicon-dioxide gets into from reactor drum 100 and collects water cooler 200 internal cooling; Cooled silicon-dioxide is gathered into micron-sized silicon-dioxide from collecting water cooler 200 entering collectors 300; Micron-sized silicon-dioxide after the gathering gets into separator 400 and carries out gas solid separation; The solid that obtains (silicon-dioxide) gets into 500 depicklings of depickling device, and the silicon-dioxide packing after the depickling is as product.
Preferably; Silicon tetrachloride as by-product of polysilicon treatment facility according to the embodiment of the invention 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.
At first the reactor drum 100 according to the silicon tetrachloride as by-product of polysilicon treatment facility of the embodiment of the invention is described below with reference to figure 2-4.
Shown in Fig. 2-4, according to embodiments of the invention, reactor drum 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 get into reaction chamber from silicon tetrachloride-gas inlet 1012, and hydrogen gets into reactor drum from hydrogen inlet 1011.
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.
According to embodiments of the invention, reactor drum 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 lower ends of the upper end of mouth body 1015 and 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, and the lower end of mouth body 1014 is provided with IT; 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.
The lower ends of sharp-tongued 1016 upper end and mouth body 1015, for example, also through 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 said 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.
Like Fig. 2-shown in Figure 4, sparger 102 comprises strut 1021 and a plurality of blades 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.It is understandable that the present invention is not limited to this, blade 1022 can be divided into the group of any suitable quantity.
As stated, sparger 102 be used to distribute silicon tetrachloride and the air-flow of air and hydrogen in the reaction chamber that enters into reactor drum 100 are avoided air-flow directly directly to rush at the bottom from reaction chamber top, thereby are improved the specific surface area that combustion conditions is controlled silicon-dioxide.
According to reactor drum 100 of the present invention, silicon tetrachloride and AIR MIXTURES get into reaction chamber from silicon tetrachloride-gas inlet 1012, and hydrogen gets into reaction chamber from hydrogen inlet 1011, flow downward after distributing through 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 drum 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 drum 100, the air pressure in the reaction chamber is lower than normal atmosphere, for example negative 1.84 kPas.
Following with reference to the collection water cooler 200 of figure 5-8 description according to the silicon tetrachloride as by-product of polysilicon treatment facility of the embodiment of the invention.
Collect water cooler 200 and link to each other, be used to cool off hydrogen chloride gas and the nano level silicon-dioxide that generates in the reaction of reactor drum 100 internal combustion with reactor drum 100.For example, collect the below that water cooler 200 can be located at reactor drum 100, hydrogen chloride gas that reactor drum 100 internal reactions generate and nano level silicon-dioxide get into 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.
As stated, reactor drum 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.The high-temp chlorination hydrogen and the silicon-dioxide that come out from reactor outlet 1013 flow in the inner chamber of water cooler opening for feed 2011 entering inner casings 201 from the top down.
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 is taper with shell 203, and more specifically, inner casing 201 is taper shape with shell 203, and the radial dimension of inner casing 201 and shell 203 reduces along direction from the top down gradually.
Like 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 spiral extension along the vertical direction.As stated, 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, revolves the upper end that body 202 can be installed to inner casing 201 through ring flange 2023, also is formed with corresponding flange in the upper end of inner casing 201; Ring flange 2023 is placed on the said 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.
Following with reference to the collector 300 of figure 9-11 description according to the silicon tetrachloride as by-product of polysilicon treatment facility of the embodiment of the invention.
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 free end that the accumulation chamber that a plurality of gathering pipes 301 link to each other successively and extend with curve form to limit, first in wherein a plurality of gathering pipes 301 are assembled pipe (nethermost gathering pipe among Fig. 9) as collector inlet 3011 and free end that last assembles pipe (the uppermost gathering pipe among Fig. 9) as collector outlet 3012.
In other words, a plurality of gathering pipes 301 join end to end successively and extend with the zigzag mode.
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 said curve form is made up of a plurality of zigzags.As shown in Figure 9, assemble pipe 301 and on the direction (above-below direction among Fig. 9) that said accumulation chamber is extended, stagger each other for adjacent two.
Preferably; Shown in Figure 10 and 11; Each is assembled pipe 301 and comprises straight-line segment and two elbow sections that are positioned at the straight-line segment two ends; Free end in said two elbow sections is respectively equipped with joint flange 302, and adjacent gathering pipe 301 links to each other through joint flange 302, links to each other thereby be convenient to a plurality of gathering pipes 301.
Shown in figure 10, preferably, first gathering pipe is managed with last gathering and is respectively equipped with gauge hatch 303, is respectively equipped with the detector (not shown) that is used to detect the interior temperature and pressure of said 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 of describing according to the silicon tetrachloride as by-product of polysilicon treatment facility of the embodiment of the invention 400.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 gets into separator 400 so that hydrogenchloride with silicon-dioxide separated from collector outlet 3012 through separator inlet with hydrogenchloride, and hydrogenchloride is discharged from pneumatic outlet, for example delivers to acid making system 600 and carries 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.
Following with reference to the depickling device 500 of figure 12-14 description according to the silicon tetrachloride as by-product of polysilicon treatment facility of the embodiment of the invention.
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, said depickling device upper part of body is provided with tail gas outlet 5014 and depickling device discharge port 5013, and the bottom of said 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 said depickling device body and stretches in the said depickling chamber.
Depickling device opening for feed 5012 links to each other with the solid outlet of separator 400, thereby gets in the depickling chambeies from depickling device opening for feed 5012 with silicon-dioxide after hydrogenchloride separates.Depickling steam is 5011 entering depickling chambeies from the depickling steam-in; 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 gets into depickling device 500 and sloughs the hydrogenchloride of 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, said 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.Top and depickling device discharge port 5013 that tail gas outlet 5014 is 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.
Like Figure 12 and 13 said, 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.
Like 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 is respectively formed on the side of furnace bottom 503 with depickling device opening for feed 5012.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.
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; Get in the depickling chamber from depickling device opening for feed 5012 with the isolating micron-sized silicon-dioxide of hydrogen chloride gas, steam is in 5011 entering depickling chambeies, depickling steam-in, and 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 that not only solves, and improved efficiency of cycling economy.In addition, according to embodiments of the invention, treating processes can be carried out under the negative pressure, between each integral part of treatment facility, flows and conveying thereby be convenient to material.
With reference to Figure 15 the treatment scheme according to the silicon tetrachloride as by-product of polysilicon of the embodiment of the invention is described below.
At first, in reactor drum 100, supply with silicon tetrachloride, hydrogen and oxygen-containing gas, silicon tetrachloride mixes with hydrogen and supplies in the reactor drum 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 drum 100, comprise first gas-solid mixture of hydrogen chloride gas and nanometer grade silica with generation.
Particularly, the temperature in the reactor drum 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 said 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 said first gas-solid mixture is introduced in the collector 300, and said nanometer grade silica is assembled through 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.
With separating in said second gas-solid mixture introducing separator 400, obtain micron silica and first tail gas that contains hydrogenchloride.As stated, separator 400 can be cyclonic separator, and for example, said second gas-solid mixture can carry out three grades of cyclonic separation and obtain said micron silica and first tail gas that contains hydrogen chloride gas.Alternatively, first tail gas after three grades of cyclonic separation can separate through the cloth bag type separator more once more.
At last, said micron-sized silicon-dioxide is introduced in the depickling device 500, removed the hydrogenchloride of said micron silica surface attachment, obtain silicon-dioxide finished product and second tail gas that contains hydrogen chloride gas to propose the depickling processing through steam gas.The specific surface area of said silicon-dioxide finished product can be about 150-380m
2Outside can packing ,/g, silicon-dioxide finished product sell.
In some embodiments of the invention, said first tail gas and second tail gas can be delivered to acid making system and prepare hydrochloric acid, and alternatively, said second tail gas can be back to separator 400 and carry out secondary separation.
Preferably, reactor drum 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, and 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, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means the concrete characteristic, structure, material or the characteristics that combine this embodiment or example to describe and is 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 characteristic, structure, material or the characteristics of description can combine with suitable manner 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: under the situation that does not break away from principle of the present invention and aim, can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited claim and equivalent thereof.
Claims (12)
1. a silicon tetrachloride as by-product of polysilicon treatment facility is characterized in that, comprising:
Reactor drum is limited with reaction chamber in the said reactor drum, and the top of said reactor drum is provided with silicon tetrachloride-gas inlet and hydrogen inlet, and the bottom that the bottom of said reactor drum is provided with ring hydrogen inlet and said reactor drum is provided with reactor outlet;
Collect water cooler; Be limited with inner chamber and the heat-eliminating medium space that is enclosed within the inner chamber outside and separates in the said collection water cooler with inner chamber; The top of said collection water cooler be provided with the water cooler opening for feed that is communicated with said inner chamber and with the heat-eliminating medium outlet of said heat-eliminating medium spatial communication; The bottom of said collection water cooler be provided with the water cooler discharge port that is communicated with said inner chamber and with the cooling medium inlet of said heat-eliminating medium spatial communication, wherein said collection water cooler is positioned at said reactor drum below so that said water cooler opening for feed links to each other with said reactor outlet;
Collector, said collector have collector inlet and collector outlet, and wherein said collector inlet links to each other with said water cooler discharge port;
Separator, said separator has separator inlet, pneumatic outlet and solid outlet, and wherein said separator inlet links to each other with said collector outlet; With
The depickling device; Be limited with the depickling chamber in the said depickling device; The top of said depickling device is provided with tail gas outlet and depickling device discharge port, and the bottom of said depickling device is provided with steam-in and depickling device opening for feed, and wherein said depickling device opening for feed links to each other with the solid outlet of said separator.
2. silicon tetrachloride as by-product of polysilicon treatment facility according to claim 1 is characterized in that, also comprises acid making system, and said acid making system links to each other with the pneumatic outlet of said separator.
3. silicon tetrachloride as by-product of polysilicon treatment facility according to claim 1 is characterized in that, the tail gas outlet of said depickling device links to each other with said separator inlet.
4. silicon tetrachloride as by-product of polysilicon treatment facility according to claim 1 is characterized in that, said separator is a three-stage cyclone separator.
5. silicon tetrachloride as by-product of polysilicon treatment facility according to claim 4 is characterized in that said separator also comprises the deep bed filter that links to each other with the last step cyclonic separator.
6. silicon tetrachloride as by-product of polysilicon treatment facility according to claim 1 is characterized in that, said reactor drum comprises:
Reactor body, said reaction chamber are limited in the said reactor body, and said silicon tetrachloride-gas inlet and hydrogen inlet are located at the top of said reactor body, and said reactor outlet is located at the bottom of said reactor body;
Muzzle, said muzzle are set in the lower end of said reactor body to limit the annular space to lower opening with said reactor body;
Link to each other with the annular space hydrogen inlet pipe of hydrogen supply in said annular space with said muzzle; With
Sparger, said sparger are arranged on and are used for uniform distribution in the said reaction chamber and supply to silicon tetrachloride-air and hydrogen in the reaction chamber from said silicon tetrachloride-gas inlet and said hydrogen inlet.
7. silicon tetrachloride as by-product of polysilicon treatment facility according to claim 6 is characterized in that, said reactor body comprises:
Mouth body, said silicon tetrachloride-gas inlet are located at said mouth body side surface and said hydrogen inlet is located at said mouth body top;
The mouth body, the lower ends of the upper end of said mouth body and said mouth body; With
Sharp-tongued, the said sharp-tongued upper end and the lower ends of said mouth body, said sharp-tongued lower end is opened wide to form said reactor outlet.
8. silicon tetrachloride as by-product of polysilicon treatment facility according to claim 1 is characterized in that, said collection water cooler comprises:
Inner casing, said inner chamber are limited in the said inner casing, and said water cooler opening for feed is located at the top of said inner casing and the bottom that said water cooler discharge port is located at said inner casing;
Shell, said shell are set in said inner casing outside, and said heat-eliminating medium space boundary is between said inner casing and shell, and said heat-eliminating medium inlet is located at the bottom of said shell and the top that the outlet of said heat-eliminating medium is located at said shell; With
Revolve body, the said body that revolves is arranged in the said heat-eliminating medium space along the vertical direction.
9. silicon tetrachloride as by-product of polysilicon treatment facility according to claim 1; It is characterized in that; Said collector comprises: a plurality of gathering pipes; Said a plurality of gathering pipe is continuous successively to limit the accumulation chamber of extending with curve form, and first in wherein said a plurality of gathering pipes assembled the free end that free end enters the mouth as said collector and last assembles pipe of pipe as said collector outlet.
10. silicon tetrachloride as by-product of polysilicon treatment facility according to claim 1 is characterized in that, said depickling device comprises:
Depickling device body, said depickling chamber are limited in the said depickling device body, and said tail gas outlet and depickling device discharge port are located at said depickling device upper part of body, and said steam-in and depickling device opening for feed are located at the bottom of said depickling device body; With
Heating tube, said heating tube are arranged on the said depickling device body and stretch in the said depickling chamber.
11. silicon tetrachloride as by-product of polysilicon treatment facility according to claim 10 is characterized in that, said depickling device body comprises:
Expanding reach, the bottom of said expanding reach are truncated cone shape, and top and said depickling device discharge port that said tail gas outlet is formed on said expanding reach are formed on the inclined-plane of said expanding reach bottom;
Shaft, the upper end of said shaft and the lower ends of said expanding reach, said heating tube is installed on the said shaft; With
Furnace bottom, the upper end of said furnace bottom link to each other with said shaft and said depickling steam-in and said depickling device opening for feed are respectively formed on the side of said furnace bottom.
12. silicon tetrachloride as by-product of polysilicon treatment facility according to claim 11; It is characterized in that; The bottom of said furnace bottom is provided with slag-drip opening; Be respectively equipped with on the side of said shaft and purge mouth and temperature-measuring port, the top and bottom of the contiguous said shaft of said purging mouth, the side of said expanding reach is provided with balance port.
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| CN111285377A (en) * | 2018-12-07 | 2020-06-16 | 新特能源股份有限公司 | System and method for producing fumed silica |
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| CN1850599A (en) * | 2006-04-29 | 2006-10-25 | 广州吉必时科技实业有限公司 | Comprehensive utilization method of by-product for poycrystalline silicon production process |
| CN201071305Y (en) * | 2007-08-06 | 2008-06-11 | 范建平 | Silicon dioxide producing device |
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| CN202054617U (en) * | 2011-03-18 | 2011-11-30 | 中国恩菲工程技术有限公司 | Equipment for processing silicon tetrachloride serving as polysilicon byproduct |
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| CN1850599A (en) * | 2006-04-29 | 2006-10-25 | 广州吉必时科技实业有限公司 | Comprehensive utilization method of by-product for poycrystalline silicon production process |
| CN201071305Y (en) * | 2007-08-06 | 2008-06-11 | 范建平 | Silicon dioxide producing device |
| CN101723384A (en) * | 2009-12-25 | 2010-06-09 | 上海竟茨环保科技有限公司 | Synthesis method and device for gas phase white carbon black |
| CN202054617U (en) * | 2011-03-18 | 2011-11-30 | 中国恩菲工程技术有限公司 | Equipment for processing silicon tetrachloride serving as polysilicon byproduct |
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Effective date of registration: 20201021 Address after: 100038 Fuxing Road 12, Beijing, Haidian District Patentee after: China Enfi Engineering Corp. Patentee after: CHINA SILICON Corp.,Ltd. Address before: 100038 Fuxing Road 12, Beijing, Haidian District Patentee before: China Enfi Engineering Corp. |
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