CN109715285A - For synthesizing the fluidized-bed reactor of trichlorosilane - Google Patents
For synthesizing the fluidized-bed reactor of trichlorosilane Download PDFInfo
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- CN109715285A CN109715285A CN201780057326.XA CN201780057326A CN109715285A CN 109715285 A CN109715285 A CN 109715285A CN 201780057326 A CN201780057326 A CN 201780057326A CN 109715285 A CN109715285 A CN 109715285A
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- Prior art keywords
- reactor
- subparticle
- fluidized
- passing valve
- separator
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- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000005052 trichlorosilane Substances 0.000 title claims abstract description 29
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 29
- 239000010703 silicon Substances 0.000 claims abstract description 29
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 11
- 238000007038 hydrochlorination reaction Methods 0.000 claims abstract description 7
- 238000012545 processing Methods 0.000 claims abstract description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 18
- 239000000956 alloy Substances 0.000 claims description 18
- 229910001293 incoloy Inorganic materials 0.000 claims description 12
- 238000005260 corrosion Methods 0.000 claims description 7
- 230000007797 corrosion Effects 0.000 claims description 7
- 229910000856 hastalloy Inorganic materials 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 37
- 230000007423 decrease Effects 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 238000000429 assembly Methods 0.000 description 2
- 230000000712 assembly Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000005243 fluidization Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000005046 Chlorosilane Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000005465 channeling Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 208000002925 dental caries Diseases 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000009491 slugging Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1872—Details of the fluidised bed reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
- B04C—APPARATUS USING FREE VORTEX FLOW, e.g. CYCLONES
- B04C3/00—Apparatus in which the axial direction of the vortex flow following a screw-thread type line remains unchanged ; Devices in which one of the two discharge ducts returns centrally through the vortex chamber, a reverse-flow vortex being prevented by bulkheads in the central discharge duct
- B04C3/04—Multiple arrangement thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
- B04C—APPARATUS USING FREE VORTEX FLOW, e.g. CYCLONES
- B04C3/00—Apparatus in which the axial direction of the vortex flow following a screw-thread type line remains unchanged ; Devices in which one of the two discharge ducts returns centrally through the vortex chamber, a reverse-flow vortex being prevented by bulkheads in the central discharge duct
- B04C3/06—Construction of inlets or outlets to the vortex chamber
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
Abstract
It is a kind of for synthesizing the fluidized-bed reactor of trichlorosilane, it includes reactor, cyclone separator, bypass line, by-passing valve and separators.There is reactor inner space react metallurgical grade silicon wherein with feed gas, reacts via hydrochlorination and direct chlorination and generates trichlorosilane gas.Cyclone separator is used for collected from metallurgical grade silicon micronized and in the increased subparticle in the inner space of reactor.Bypass line is connected to reactor, for subparticle to be discharged to the outside of reactor.By-passing valve is set in bypass line.Separator is connected to discharge gas separation and processing of the by-passing valve for subparticle autoreactor to be discharged.
Description
Technical field
The present invention provides a kind of for synthesizing the fluidized-bed reactor of trichlorosilane, metallurgical grade silicon can be used and via hydrogen
Chlorination reaction (hydrochlorination reaction) and direct chlorination react (direct chlorination
Reaction) trichlorosilane gas is generated.
Background technique
In known technology, when metallurgical grade silicon has 98% to 99% purity, hydrochlorination is carried out
(hydrochlorination reaction) and direct chlorination react (direct chlorination reaction), energy
Enough generate trichlorosilane.(Siemens chemical vapor deposition is reacted using Siemens's chemical deposition
Reaction), it is 9N to 11N or the higher high-purity polycrystalline silicon of purity that trichlorosilane, which is for generating purity,.
Fluidized-bed reactor can be used to synthesize trichlorosilane gas.Fluidized-bed reactor has the stream that can utilize particle
Move make interior temperature remain unchanged and can using increase solid contact between gas come the advantages of promoting yield.However, stream
Fluidized bed reactor has the shortcomings that operation and maintenance are not easy.
Trichlorosilane can be generated when metallurgical grade silicon is completed to react in the reactor with feed gas.So far, metallurgical grade silicon
It by micronized (micronized) and can be built up in the reactor as the time carries out.
A small amount of subparticle has front for smooth flow (smooth flow) characteristic of metallurgical grade silicon in reactor
Influence, but when subparticle is excessively accumulated, it may occur that channel (channeling) or plug flow (slugging)
Phenomenon.
Contacting efficiency (contact efficiency) meeting when channel or plug flow phenomenon occur, between gas and solid
Decline, has negative impact for reactivity.Furthermore when being accumulated in the reactor without reactive subparticle, three
The yield of chlorosilane will be led to the problem of.
In this regard, needing to remove the subparticle of accumulation in the reactor.However, since the characteristic of reactor is by feeding gas
Body is dispensed by the lower part of reactor into therefore the small subparticle of size will be raised to the upper part of reactor and again
Via collected by cyclone separator, then via in material returning device (dipleg) Returning reactor.
A small amount of not collected by reactor, subparticle can be discharged outside reactor, but be discharged the micro- of reactor
Fine grain quantity can be less than the quantity for accumulating subparticle in the reactor.That is, because subparticle can react
It is accumulated in device, as the operating time of reactor is longer, the stability of fluidized-bed reactor is more bad.
Therefore, in order to remove accumulation subparticle in the reactor, it is necessary to which shut down fluidized-bed reactor, causes
Yield decline and economic loss.In order to remove subparticle and avoid above-mentioned loss simultaneously, other than cyclone separator,
Also need in addition to provide the device of discharge and control subparticle and the device of the subparticle for separating and handling discharge.
Summary of the invention
Technical problem
The present invention provide it is a kind of for synthesizing the fluidized-bed reactor of trichlorosilane, can by metallurgical grade silicon carry out hydrogen chlorine
Change reaction and direct chlorination reaction and generates trichlorosilane.
Furthermore the present invention provide it is a kind of for synthesizing the fluidized-bed reactor of trichlorosilane, when synthesizing trichlorosilane,
The subparticle generated in reactor can be removed to reactor.
Technical solution
One embodiment of the invention is provided for synthesizing the fluidized-bed reactor of trichlorosilane, wherein including: reactor,
With inner space, react metallurgical grade silicon wherein with feed gas, it is anti-via hydrochlorination and direct chlorination
It answers and generates trichlorosilane gas；Cyclone separator, for collected from metallurgical grade silicon micronized and in the inner space of reactor
The subparticle being lifted；Bypass line is connected to the reactor, for the subparticle to be discharged to the reactor
Outside；By-passing valve is set in the bypass line；And separator, it is connected to the by-passing valve, being used for will be described fine
The separation of discharge gas and processing that particle is discharged from the reactor.
The aperture (opening degree) of the adjustable bypass line of by-passing valve.
Charging area (inlet of the opening area (opening area, OA) of by-passing valve to the cyclone separator
Area, IA) ratio (OA:IA) be 1 to 1,1 to 5 and 1 to 10 one of them (OA:IA=1:1,1:5 or 1:10).
The material of bypass line and by-passing valve have high corrosion resistance and can be selected from by 800 alloy of Incoloy,
Made by the one of which of Incoloy 800H alloy and Hastelloy alloy.
Separator may include: cavity is connected to bypass line；Cyclone separator is set in the cavity；And filtering
Device is set to the feed lines of the cyclone separator.
The filter that the separator is included can be selected from wherein the one of vertical filter, horizon-lai filters and ceramic membrane
Kind.
The material of separator have high corrosion resistance, and selected from by 800 alloy of Incoloy, Incoloy 800H alloy with
And made by the one of which of Hastelloy alloy.
Invention effect
An embodiment according to the present invention, it is micro- from metallurgical grade silicon in the inner space of reactor when synthesizing trichlorosilane
Granulated subparticle can be discharged to the outside of reactor, remove subparticle whereby, therefore stabilization fluid bed can react
Device.Furthermore it is possible to avoid the fluidized-bed reactor that shuts down, whereby, the running time can extend, the yield of trichlorosilane gas
It can be enhanced with the flow behavior of metallurgical grade silicon, cost can also decline.
Furthermore in later process stages because in reactor there are subparticle and there may be the problem of can also be because
This is avoided by.
Detailed description of the invention
The structure that Fig. 1 show the fluidized-bed reactor for synthesizing trichlorosilane of an exemplary embodiment of the invention is shown
It is intended to.
Specific embodiment
The embodiment of the present invention is enumerated in detailed below, and attached drawing is cooperated to be described in detail, so that technical field is common
Technical staff can realize the present invention accordingly.Person of an ordinary skill in the technical field should be appreciated that the number that the present invention is lifted
Disclosed embodiment can be adjusted under the spirit for not departing from this exposure to realize this by a embodiment in different ways
Invention.
It is noted that attached drawing is simplified schematic diagram, the present invention is not limited with this.Also, in addition with symbol in attached drawing
Number cooperation illustrates various assemblies described in the specification.
In addition, for convenience of explanation, the size and thickness of various assemblies are not drawn in attached drawing of the invention with equal proportion,
And the contents of the present invention are not limited to content shown in the drawings.
When claiming a component to be connected to another component in the present specification comprising the feelings that these components are connected to each other directly
Condition, it is also possible to include the case where being additionally provided with being indirectly connected with for other elements between these components.Furthermore in the present specification,
When other contrary circumstances are not particularly described out, " comprising/include any device/component " can be understood as these devices/
The presence of component, but it is not excluded for other device/component presence.
The structure that Fig. 1 show the fluidized-bed reactor for synthesizing trichlorosilane of an exemplary embodiment of the invention is shown
It is intended to.As shown in Figure 1, the fluidized-bed reactor for synthesizing trichlorosilane of an exemplary embodiment of the invention (all claims below
For fluidized-bed reactor) it include reactor 10, cyclone separator 20, bypass line 30, by-passing valve 40 and separator 50.
Reactor 10 has inner space, will do it reaction wherein.Metallurgical grade silicon and feed gas can be in the inside
Space via hydrogen chloride (hydrochlorination) react and direct chlorination (direct chlorination) reaction and
Trichlorosilane gas is generated, and as the time generates the subparticle P of micronized.
For example, by metallurgical grade silicon supplied to (not shown) in the inner space of reactor 10, and fluidised form will to be used for
The feed gas for changing (fluidizing) metallurgical grade silicon is supplied in reactor 10.Feed gas from the lower part of reactor 10 toward
Upper supply, so that metallurgical grade silicon fluidization.
When synthesizing trichlorosilane, the subparticle P of inner space can be lifted in reactor 10.It is interior in reactor 10
Portion space is provided with cyclone separator 20, and for collecting the subparticle P being lifted in inner space, and part is not collected
Subparticle P heat exchanger 60 is discharged to by the first pumping-out line 61.
Subparticle P collected by feed lines 21 via cyclone separator 20 can be via connection cyclone separator 20
Material returning device 22 and send the inner space of reactor 10 back to, therefore these subparticles P can be reused and carry out metallurgical grade silicon
Fluidisation.
Bypass line 30 connects the upper part of reactor 10, the subparticle P row for will be lifted in inner space
It is arrived except reactor 10 out.That is, bypass line 30 and cyclone separator 20 can be collected when synthesizing trichlorosilane
Subparticle P in the upper part of reactor 10, to remove subparticle P.
By-passing valve 40 is provided in bypass line 30, whereby, when needing to be discharged subparticle P, via on/off operation
And aperture (opening degree) adjustment operation, the ON/OFF and aperture of adjustable bypass line 30.It whereby, can be with
It does not need to stop operating reactor 10 and subparticle P can also continuously be discharged.
Therefore, can extend for synthesizing the operating time of the reactor 10 of trichlorosilane, the yield of trichlorosilane can
It is elevated, cost can also decline.
For example, bypass line 30 and by-passing valve 40 can by with high corrosion resistance 800 alloy of Incoloy,
Made by Incoloy 800H alloy or Hastelloy alloy.Therefore, discharge gas and subparticle can be effectively prevented
Corrosion for bypass line 30 and by-passing valve 40.
Meanwhile the opening area (opening area, OA) of by-passing valve 40 is to the charging area of cyclone separator 20
The ratio (OA:IA) of (inlet area, IA) is 1 to 1,1 to 5 and 1 to 10 one of them.
That is, subparticle P can be introduced into cyclone separator 20 or be moved to the by-passing valve 40 on top.Drawn
The most of subparticle P for entering the feed lines 21 of cyclone separator 20 can be collected and return in reactor 10, but portion
Divide subparticle P that can not be collected into and scatter and disappear, therefore can be discharged by the first pumping-out line 61.At the same time, it is moved
The subparticle P of supreme radical port valve 40 can be discharged to outside reactor 10 via bypass line 30.Separator 50 and side
Subparticle P in discharge gas of the connection of port valve 40 to separate and handle the discharge of autoreactor 10.
Bypass line 30 and by-passing valve 40 in the inner space of reactor 10 can be separated with cyclone separator 20
Setting, to adjust the discharge rate of the subparticle P of the discharge of autoreactor 10.That is, by-passing valve 40 adjustable fine
The cumulative speed of subparticle P in the rate of discharge to more than reactor 10 of grain P.
As above-mentioned, since subparticle P can be removed in bypass line 30, by-passing valve 40 and separator 50, wherein fine
It is unstable and do not have reactivity, therefore energy that particle P will cause the metallurgical grade silicon flow behavior in 10 inner space of reactor
Reactor 10 is enough set to extend operation and be not necessary to stop operating.It whereby, can be to avoid the economy caused by reactor 10 that stops operating
Loss.
The rate of discharge of subparticle P is controlled via adjustment aperture, it is empty that by-passing valve 40 can stablize 10 inside of reactor
Between in metallurgical grade silicon flow behavior.Therefore, unnecessary yield can be reduced via the rate of discharge of control subparticle P
Loss.
For example, separator 50 may include the cavity 51 for being connected to bypass line 30, the whirlwind being arranged in cavity 51
Separator 52 and be arranged in cyclone separator 52 feed lines filter 53.
Therefore, it can be set included in discharge gas by the subparticle P that bypass line 30 is introduced into separator 50
The filter 53 set in the feed lines of cyclone separator 52 is filtered, and is collected in cavity 51.
For example, filter 53 can be made of vertical filter, horizon-lai filters or ceramic membrane, depend on whirlwind
The position of the feed lines of separator 52.
For example, separator 50 have high corrosion resistance and by 800 alloy of Incoloy, Incoloy 800H alloy or
Made by Hastelloy alloy.Therefore, the corruption of discharge gas and subparticle P for separator 50 can be effectively prevented
Erosion.
The discharge of subparticle P from metallurgical grade silicon micronized and in the formation of the inner space of reactor 10 can be via control
The opening area of by-passing valve 40 processed determines.It therefore, just will not be in the inside of reactor 10 without reactive subparticle P
It is accumulated in space, or the subparticle P accumulated is in the range of the flow behavior of metallurgical grade silicon is not suppressed.
An exemplary embodiment according to the present invention, fluidized-bed reactor also include to be connected in 10 inner space of reactor
Cyclone separator 20 and separator 50 heat exchanger 60.
Therefore, cyclone separator 20 is connected to heat exchanger 60 via the first pumping-out line 61.In subparticle P by whirlwind
After separator 20 is collected, the high temperature exhaust gas comprising the subparticle P not being collected partially can pass through first row outlet
Road 61 is discharged to heat exchanger 60.
Separator 50 is connected to heat exchanger 60 via the second pumping-out line 62.It is separated in subparticle P by separator 50
And after processing, high temperature exhaust gas can be discharged to heat exchanger 60 by the second pumping-out line 62.
It is provided in second pumping-out line 62 backflow preventer 63 (backflow prevention valve), therefore when height
Temperature discharge gas is when being discharged to the second pumping-out line 62, can be avoided from the first pumping-out line 61 and heat exchanger 60
High temperature exhaust gas flows backward to the second pumping-out line 62.
In addition, pump 64 is connected to the end of heat exchanger 60.When high temperature exhaust gas passes through the first pumping-out line 61, second
When pumping-out line 62 and heat exchanger 60, pump 64 is discharged from the cooling quenching gas (quenching of high temperature exhaust gas
gas)。
As above-mentioned, since subparticle P is separately processed in separator 50, it is avoided that after reactor 10
May be because of subparticle P in continuous operation stage structure (such as heat exchanger 60 and pump 64 etc.) the problem that.
For example, according to an exemplary embodiment, when fluidized-bed reactor synthesizes trichlorosilane, reactor 10 it is interior
The upper part in portion space will certainly have the subparticle P of distribution.In that case, it is arranged from the bypass line 30 of reactor 10
The quantity of subparticle P out is adjusted via the opening area of adjustment by-passing valve 40.It is described above can be via following experiment
Illustration is real.
The first experimental example is please referred to, when the flowing speed of metallurgical grade silicon and feed gas in the inner space of reactor 10
Rate is 0.1m/s, and the opening area (OA) of by-passing valve 40 to the area ratio of the charging area (IA) of cyclone separator 20 (OA:
IA) when being 1:1, subparticle P is 8.75g/min by the rate of discharge of by-passing valve 40.
The second experimental example is please referred to, when the flowing speed of metallurgical grade silicon and feed gas in the inner space of reactor 10
Rate is 0.1m/s, and the opening area of by-passing valve 40 is 1:5 to the area ratio (OA:IA) of the charging area of cyclone separator
When, the rate of discharge that subparticle P passes through by-passing valve 40 is 1.67g/min.
Third experimental example is please referred to, when the flowing speed of metallurgical grade silicon and feed gas in the inner space of reactor 10
Rate is 0.1m/s, and the opening area of by-passing valve 40 is 1:10 to the area ratio (OA:IA) of the charging area of cyclone separator
When, the rate of discharge that subparticle P passes through by-passing valve 40 is 0.3g/min.
With reference to the first experimental example to third experimental example, it is to be understood that at identical flow rate (0.1m/s), work as area
When ratio (OA:IA) rises, compared to charging area (IA), opening area (OA) can decline, and subparticle P passes through by-passing valve
40 rate of discharge can decline.
The 4th experimental example is please referred to, when the flowing speed of metallurgical grade silicon and feed gas in the inner space of reactor 10
Rate is 0.15m/s, and the opening area of by-passing valve 40 is 1:1 to the area ratio (OA:IA) of the charging area of cyclone separator
When, the rate of discharge that subparticle P passes through by-passing valve 40 is 25g/min.
The 5th experimental example is please referred to, when the flowing speed of metallurgical grade silicon and feed gas in the inner space of reactor 10
Rate is 0.15m/s, and the opening area of by-passing valve 40 is 1:5 to the area ratio (OA:IA) of the charging area of cyclone separator
When, the rate of discharge that subparticle P passes through by-passing valve 40 is 8.33g/min.
The 6th experimental example is please referred to, when the flowing speed of metallurgical grade silicon and feed gas in the inner space of reactor 10
Rate is 0.15m/s, and the opening area of by-passing valve 40 is 1:10 to the area ratio (OA:IA) of the charging area of cyclone separator
When, the rate of discharge that subparticle P passes through by-passing valve 40 is 1.6g/min.
With reference to the 4th experimental example to the 6th experimental example, it is to be understood that at identical flow rate (0.15m/s), work as area
When ratio (OA:IA) rises, compared to charging area (IA), the ratio regular meeting decline of opening area (OA), and subparticle P passes through
The rate of discharge of by-passing valve 40 can decline.
In the first experimental example into third experimental example, flow rate 0.1m/s, in the 4th experimental example to the 6th experimental example,
Flow rate is 0.15m/s.From the above, it is to be understood that rise to when flow rate, the rate of discharge of subparticle P has
It is significant different.
Under the general operation of fluidized-bed reactor, the state that maintains backflow preventer 63 and by-passing valve 40 to simultaneously close off.
Separator 50 maintains and the identical internal pressure of reactor 10.That is, when not needing discharge subparticle P, it is most of
Subparticle P collected by cyclone separator 20 can be recycled (re-circulated) in the interior space.
When needing to be discharged subparticle P, the by-passing valve 40 and backflow preventer 63 of reactor 10 are opened simultaneously, are discharged whereby
Gas forms the fluid for flowing to separator 50.Therefore, subparticle P is discharged to the outside of reactor 10.
Here, heat exchanger 60 is operated in the case where pressure is less than 10 about 1 to 2 bars of reactor (bar).Therefore, it is discharged
High temperature exhaust gas to separator 50 is provided to heat exchanger 60 by the second pumping-out line 62 and backflow preventer 63.Pump
64 operate in the case where pressure is less than 60 about 1 to 2 bars of heat exchanger (bar).Depending on the driving of pump 64, in heat exchanger 60
The quenching gas cooled down can be to be discharged in automatic heat-exchanger 60.
It is fully drained in subparticle P autoreactor 10 to separator 50, via closing backflow preventer 63 to hinder
It is discharged every discharge gas.Then, via the by-passing valve 40 for closing reactor 10 to obstruct discharge gas and subparticle P quilt
Discharge.
The foregoing is merely exemplary embodiments of the invention, are not intended to restrict the invention, for this field
For technical staff, the invention may be variously modified and varied.It is done within the spirit and principles of the present invention any
Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Symbol description
10 reactors
20 cyclone separators
21 feed lines
30 bypass lines
40 by-passing valves
50 separators
51 cavitys
52 cyclone separators
53 filters
60 heat exchangers
61 first pumping-out lines
62 second pumping-out lines
63 backflow preventers
64 pumps
IA feeds area
OA opening area
P subparticle
Claims (7)
1. a kind of fluidized-bed reactor, for synthesizing trichlorosilane, the fluidized-bed reactor includes:
There is reactor inner space react metallurgical grade silicon wherein with feed gas, via hydrochlorination and
Direct chlorination reacts and generates trichlorosilane gas；
Cyclone separator, for being lifted collected from the metallurgical grade silicon micronized and in the inner space of the reactor
Subparticle；
Bypass line is connected to the reactor, for the subparticle to be discharged to the outside of the reactor；
By-passing valve is set in the bypass line；And
Separator is connected to the by-passing valve, for separating the subparticle from the discharge gas that the reactor is discharged
With processing.
2. fluidized-bed reactor according to claim 1, wherein
The aperture of the adjustable bypass line of by-passing valve.
3. fluidized-bed reactor according to claim 2, wherein
The opening area of the by-passing valve to the ratio (OA:IA) of the charging area of the cyclone separator be 1 to 1,1 to 5 with
And 1 to 10 one of them.
4. fluidized-bed reactor according to claim 1, wherein
The material of the bypass line and the by-passing valve has high corrosion resistance and by 800 alloy of Incoloy, Incoloy
Made by the one of which of 800H alloy and Hastelloy alloy.
5. fluidized-bed reactor according to claim 1, wherein
The separator includes:
Cavity is connected to the bypass line；
Cyclone separator is set in the cavity；And
Filter is set to the feed lines of the cyclone separator.
6. fluidized-bed reactor according to claim 1, wherein
The separator includes filter, and the filter is selected from vertical filter, horizon-lai filters and ceramic membrane
It is one of.
7. fluidized-bed reactor according to claim 1, wherein
The material of the separator have high corrosion resistance, and by 800 alloy of Incoloy, Incoloy 800H alloy and
Made by the one of which of Hastelloy alloy.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR10-2016-0119376 | 2016-09-19 | ||
| KR1020160119376A KR101987129B1 (en) | 2016-09-19 | 2016-09-19 | Fluidized bed reactor for composing trichlorosilane |
| PCT/KR2017/010205 WO2018052262A1 (en) | 2016-09-19 | 2017-09-18 | Fluidized bed reactor for synthesizing trichlorosilane |
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| KR (1) | KR101987129B1 (en) |
| CN (1) | CN109715285A (en) |
| TW (1) | TWI681817B (en) |
| WO (1) | WO2018052262A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110342524A (en) * | 2019-08-19 | 2019-10-18 | 新疆协鑫新能源材料科技有限公司 | A kind of fine silica powder subregion reaction fluidized bed and method |
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| KR102587565B1 (en) * | 2021-11-15 | 2023-10-12 | 한국에너지기술연구원 | System and Method for contrilling intenal gas flow velocity of fluidized bed using section area changes |
| CN115430370B (en) * | 2022-09-30 | 2023-10-20 | 浙江开化合成材料有限公司 | Chlorosilane synthesizer |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1382690A (en) * | 2001-04-12 | 2002-12-04 | 瓦克化学有限公司 | Dust circulation when directly synthetizing silane chhloride and silane methyl chloride in fluidized bed |
| KR100436095B1 (en) * | 1995-11-14 | 2004-09-13 | 가부시키가이샤 도쿠야마 | Cyclone and Fluidized Bed Reactor with the Same |
| CN101124434A (en) * | 2004-10-13 | 2008-02-13 | 福斯特能源公司 | Cyclone bypass for a circulating fluidized bed reactor |
| KR101133658B1 (en) * | 2009-02-09 | 2012-04-10 | 코아텍주식회사 | A Manufacturing Method and A Manufacturing Apparatus of TrichlorosilaneSiHCl3 using the Metal Catalyst |
| CN102653405A (en) * | 2012-04-20 | 2012-09-05 | 中国恩菲工程技术有限公司 | Device for treating hydrogenated by-product of silicon tetrachloride |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100661284B1 (en) * | 2006-02-14 | 2006-12-27 | 한국화학연구원 | Preparation of granular polycrystalline using fluidized bed reactor |
| JP5316290B2 (en) * | 2008-08-05 | 2013-10-16 | 三菱マテリアル株式会社 | Trichlorosilane production apparatus and production method |
| KR101545201B1 (en) * | 2008-10-16 | 2015-08-19 | 주식회사 케이씨씨 | Thermal plasma fluidized bed reactor and method for preparing polysilicon using the same |
| DE102009037155B3 (en) * | 2009-08-04 | 2010-11-04 | Schmid Silicon Technology Gmbh | Process and plant for the production of trichlorosilane |
| KR20130027445A (en) * | 2011-09-07 | 2013-03-15 | 주식회사 엘지화학 | Cyclone having property of adjusting bubble size and fluidized bed reactor comprising the same |
| KR101505731B1 (en) * | 2013-07-16 | 2015-03-24 | 웅진에너지 주식회사 | A Gas Exhaust Pipe for Fluidized Bed Reactor |
-
2016
- 2016-09-19 KR KR1020160119376A patent/KR101987129B1/en active IP Right Grant
-
2017
- 2017-09-18 CN CN201780057326.XA patent/CN109715285A/en active Pending
- 2017-09-18 WO PCT/KR2017/010205 patent/WO2018052262A1/en active Application Filing
- 2017-09-19 TW TW106132073A patent/TWI681817B/en active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100436095B1 (en) * | 1995-11-14 | 2004-09-13 | 가부시키가이샤 도쿠야마 | Cyclone and Fluidized Bed Reactor with the Same |
| CN1382690A (en) * | 2001-04-12 | 2002-12-04 | 瓦克化学有限公司 | Dust circulation when directly synthetizing silane chhloride and silane methyl chloride in fluidized bed |
| CN101124434A (en) * | 2004-10-13 | 2008-02-13 | 福斯特能源公司 | Cyclone bypass for a circulating fluidized bed reactor |
| KR101133658B1 (en) * | 2009-02-09 | 2012-04-10 | 코아텍주식회사 | A Manufacturing Method and A Manufacturing Apparatus of TrichlorosilaneSiHCl3 using the Metal Catalyst |
| CN102653405A (en) * | 2012-04-20 | 2012-09-05 | 中国恩菲工程技术有限公司 | Device for treating hydrogenated by-product of silicon tetrachloride |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110342524A (en) * | 2019-08-19 | 2019-10-18 | 新疆协鑫新能源材料科技有限公司 | A kind of fine silica powder subregion reaction fluidized bed and method |
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| Publication number | Publication date |
|---|---|
| KR20180031226A (en) | 2018-03-28 |
| WO2018052262A1 (en) | 2018-03-22 |
| KR101987129B1 (en) | 2019-06-10 |
| TWI681817B (en) | 2020-01-11 |
| TW201821156A (en) | 2018-06-16 |
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