CN204138354U - The device of trichlorosilane prepared by plasma heating fluidized-bed - Google Patents
The device of trichlorosilane prepared by plasma heating fluidized-bed Download PDFInfo
- Publication number
- CN204138354U CN204138354U CN201420589670.7U CN201420589670U CN204138354U CN 204138354 U CN204138354 U CN 204138354U CN 201420589670 U CN201420589670 U CN 201420589670U CN 204138354 U CN204138354 U CN 204138354U
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- CN
- China
- Prior art keywords
- fluidized
- bed reactor
- plasma
- hydrogen
- silicon tetrachloride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 238000010438 heat treatment Methods 0.000 title claims abstract description 26
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000005052 trichlorosilane Substances 0.000 title claims abstract description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 40
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims abstract description 37
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 37
- 239000001257 hydrogen Substances 0.000 claims abstract description 33
- 239000007789 gas Substances 0.000 claims abstract description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000006200 vaporizer Substances 0.000 claims abstract description 10
- 235000013312 flour Nutrition 0.000 claims abstract description 9
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000005855 radiation Effects 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005259 measurement Methods 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 3
- 238000005265 energy consumption Methods 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 235000013339 cereals Nutrition 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- 230000009466 transformation Effects 0.000 description 7
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 5
- 229920005591 polysilicon Polymers 0.000 description 5
- 238000007323 disproportionation reaction Methods 0.000 description 4
- 238000005984 hydrogenation reaction Methods 0.000 description 4
- 230000008016 vaporization Effects 0.000 description 4
- 238000009834 vaporization Methods 0.000 description 4
- 238000005485 electric heating Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000001360 synchronised effect Effects 0.000 description 2
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 229940045803 cuprous chloride Drugs 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The utility model relates to the device that trichlorosilane prepared by a kind of plasma heating fluidized-bed, comprise: fluidized-bed reactor (10), hot water radiation wire (8) is provided with in fluidized-bed reactor (10), fluidized-bed reactor (10) wall is provided with silica flour charging opening (11), measurement and control of temperature mouth (12) and pressure warning unit (9), fluidized-bed reactor (10) bottom is provided with plasma gun (3) and hydrogen and silicon tetrachloride gas mixer (6), plasma gun (3) is connected with plasma heat source body (2), plasma heat source body (2) is connected with plasma power supply working gas entrance (1), hydrogen is connected with vaporizer (14) with hydrogen inlet (4) with silicon tetrachloride gas mixer (6), vaporizer (14) is provided with silicon tetrachloride entrance (5), fluidized-bed reactor (10) top is provided with offgas outlet (13).The utility model improves the thermograde in fluidized-bed reactor, makes to obtain thermal field in fluidized-bed reactor even, provides hydrogen plasma, significantly improve converting silicon tetrachloride rate, reduce energy consumption.
Description
Technical field
The utility model relates to the device that trichlorosilane prepared by a kind of plasma heating fluidized-bed.Belong to polysilicon preparing technical field.
Background technology
Current global polysilicon enterprise, more than 80% employing improved Siemens.Improved Siemens produces polysilicon, inevitably produces a large amount of silicon tetrachloride.In order to realize falling this consumption reduction, domestic early stage project generally adopts hot hydrogenation process to be trichlorosilane by converting silicon tetrachloride, and concrete reactional equation is as follows:
SiCl
4+ H
2→ SiHCl
3+ HCl
The temperature of reaction of this reaction is 1150 DEG C ~ 1250 DEG C, reaction pressure 0MPa(G) ~ 0.6MPa(G).
Hot hydrogenation process mainly adopts bell-jar reactor, reach between surface temperature 1200 DEG C ~ 1300 DEG C by giving electric heating part heating power, due to electric heating part finite surface area, cause that the thermograde in bell-jar reactor is large, thermal field is uneven, silicon tetrachloride and hydrogen generate trichlorosilane in electric heating part surface reaction, low conversion rate (less than 20%), simultaneously in order to keep higher conversion, adopt less inlet amount, heat utilization ratio is low, the higher (2.0 ~ 3.0kWh/kg-SiCl of energy consumption
4).
In recent years, in order to reduce production of polysilicon cost, domestic polysilicon enterprise has brought into use cold hydrogenation process processing silicon chloride, prepares trichlorosilane by hydrogen, silica flour disproportionation reduction silicon tetrachloride.Concrete reactional equation is as follows:
3SiCl
4+ 2H
2+ Si → 4SiHCl
3
The temperature of reaction of this reaction is 450 DEG C ~ 550 DEG C, reaction pressure 1.5MPa(G) ~ 3.5MPa(G).
Cuprous chloride is catalyzer.
The fluidized-bed reactor that cold hydrogenation process mainly adopts inner bag to heat, maintaining temperature in fluidized-bed reactor by giving inner bag heating power is 450 DEG C ~ 550 DEG C, transformation efficiency higher (20% ~ 23%), and treatment capacity is larger, heat utilization rate is higher, the lower (0.5 ~ 1.5kWh/kg-SiCl of energy consumption
4).But owing to being heated by ecto-entad, still there is the problem that thermograde is comparatively large, thermal field is uneven, transformation efficiency is lower, energy consumption is higher in fluidized-bed reactor.
Utility model content
The purpose of this utility model is to overcome above-mentioned deficiency, provide a kind of and make that the thermograde in fluidized-bed reactor is less, thermal field evenly, significantly improve converting silicon tetrachloride rate, reduce the device that the plasma heating fluidized-bed of energy consumption prepares trichlorosilane.
The purpose of this utility model is achieved in that the device of trichlorosilane prepared by a kind of plasma heating fluidized-bed, comprise: fluidized-bed reactor, hot water radiation wire is provided with in fluidized-bed reactor, fluidized-bed reactor wall is provided with silica flour charging opening, measurement and control of temperature mouth and pressure warning unit, plasma gun and hydrogen and silicon tetrachloride gas mixer is provided with bottom fluidized-bed reactor, plasma gun is connected with plasma heat source body, plasma heat source body is connected with plasma power supply working gas entrance, hydrogen is connected with vaporizer with hydrogen inlet with silicon tetrachloride gas mixer, vaporizer is provided with silicon tetrachloride entrance, heating agent entrance and heating agent outlet, fluidized-bed reactor top is provided with offgas outlet.
Trichlorosilane is prepared with the fluidized-bed reactor of plasma heating, heat-exchange equipment can be reduced, reduce equipment failure, effective thermograde improved in fluidized-bed reactor, make thermal field in fluidized-bed reactor evenly, effectively utilize the space in fluidized-bed reaction, reduce energy expenditure, improve transformation efficiency, the more important thing is that hydrogen plasma can strengthen reaction, transformation efficiency is significantly improved.And the copper chloride catalyst of meeting pollution products need not be used.
The beneficial effects of the utility model:
The utility model reduces silicon tetrachloride superheater and the hydrogen well heater that equipment failure mainly decreases vaporization, decrease silicon tetrachloride superheater to break down, save energy mainly because plasma gas is direct and grain silicon interacts, and they are heated to temperature of reaction, and do not have reactor wall to intercept in the middle of this, reduce energy consumption; Improve the thermal field of transformation efficiency mainly on the one hand in fluidized-bed reactor evenly, effectively utilize the space in fluidized-bed reaction, improve transformation efficiency, the more important thing is that hydrogen plasma can strengthen reaction, transformation efficiency is significantly improved.
Accompanying drawing explanation
In order to be illustrated more clearly in the utility model embodiment or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only embodiments more of the present utility model, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the overall structure schematic diagram that the device of trichlorosilane prepared by the utility model plasma heating fluidized-bed.
Reference numeral in figure:
Plasma power supply working gas entrance 1
Plasma heat source body 2
Plasma gun 3
Hydrogen inlet 4
Silicon tetrachloride entrance 5
Hydrogen and silicon tetrachloride gas mixer 6
Thermal insulation layer 7
Hot water radiation wire 8
Pressure warning unit 9
Fluidized-bed reactor 10
Silica flour charging opening 11
Measurement and control of temperature 12
Offgas outlet 13
Vaporizer 14
Heating agent entrance 15
Heating agent outlet 16.
Embodiment
In order to understand the utility model further, below in conjunction with embodiment, the utility model preferred implementation is described, but should be appreciated that these describe just in order to further illustrate feature and advantage of the present utility model, instead of the restriction to the utility model claim.
The utility model provides and reduces silicon tetrachloride by hydrogen and silica flour disproportionation in a fluidized bed reactor by plasma heating and prepare trichlorosilane, its Synchronous Heating through vaporization silicon tetrachloride and hydrogen make-up mixed gas, reduce heat-exchange equipment, reduce equipment failure; Improve the thermograde in fluidized-bed reactor, make the thermal field in fluidized-bed reactor even; Hydrogen plasma is provided, significantly improves converting silicon tetrachloride rate, reduce energy consumption.
Below in conjunction with the accompanying drawing in the utility model embodiment, be clearly and completely described the technical scheme in the utility model embodiment, obviously, described embodiment is only the utility model part embodiment, instead of whole embodiments.Based on the embodiment in the utility model, those of ordinary skill in the art are not making the every other embodiment obtained under creative work prerequisite, all belong to the scope of the utility model protection.
As shown in Figure 1,
The utility model relates to the device that trichlorosilane prepared by a kind of plasma heating fluidized-bed, described device comprises: fluidized-bed reactor 10, hot water radiation wire 8 is provided with in fluidized-bed reactor 10, fluidized-bed reactor 10 wall is provided with silica flour charging opening 11, measurement and control of temperature mouth 12 and pressure warning unit 9, fluidized-bed reactor 10 is outside equipped with thermal insulation layer 7, plasma gun 3 and hydrogen and silicon tetrachloride gas mixer 6 is provided with bottom fluidized-bed reactor 10, plasma gun 3 is connected with plasma heat source body 2, plasma heat source body 2 is connected with plasma power supply working gas entrance 1, hydrogen is connected with vaporizer 14 with hydrogen inlet 4 with silicon tetrachloride gas mixer 6, vaporizer 14 is provided with silicon tetrachloride entrance 5, heating agent entrance 15 and heating agent outlet 16, fluidized-bed reactor 10 top is provided with offgas outlet 13.
The utility model provides and reduces silicon tetrachloride by hydrogen and silica flour disproportionation in a fluidized bed reactor by plasma heating and prepare trichlorosilane, and it comprises following processing step:
Step one, add silicon grain to fluidized-bed reactor 10, with rare gas element as nitrogen carries out gas displacement;
Step 2, in fluidized-bed reactor 10, pass into hydrogen set up a silicon grain fluidized-bed;
Step 3, be energized preheating silicon grain fluidized-bed to hot water radiation wire 8;
Step 4, in plasma heat source body 2, pass into plasma power supply working gas as hydrogen, its plasma is changed into high temperature plasma gas, form hydrogen plasma, high temperature plasma gas is directly imported bottom fluidized-bed reactor, passes into the preheating together of silicon grain fluidized-bed;
Step 5, by measurement and control of temperature 12 observing and controlling silicon grain fluidized-bed temperature, when silicon grain temperature reaches 200 DEG C ~ 1300 DEG C, stop being energized to hot water radiation wire 8;
Step 6, liquid silicon tetrachloride to be vaporized in vaporizer 14;
Step 7, by hydrogen make-up and vaporization after liquid silicon tetrachloride mix in hydrogen and silicon tetrachloride gas mixer 6, and regulate hydrogen make-up flow, between the proportioning 0.1:1 ~ 10:1 making hydrogen and silicon tetrachloride, control simultaneously hydrogen plasma, hydrogen make-up and silicon tetrachloride mixed gas enter fluidized-bed reactor 10 before temperature be in 200 DEG C ~ 1300 DEG C; Maintain silicon grain temperature between 200 DEG C ~ 1300 DEG C, pressure is 0MPa(G) ~ 3.5MPa(G);
Step 8, hydrogen plasma, hydrogen make-up and silicon tetrachloride mixed gas enter in fluidized-bed reactor 10, react produce trichlorosilane gas with silicon grain, form tail gas with the silicon tetrachloride of non-complete reaction together with mixed gas of hydrogen etc.;
Step 9, by tail gas take out, be separated, prepare trichlorosilane; Unreacted is silicon tetrachloride and hydrogen recovery recycle completely.
The utility model provides and reduces silicon tetrachloride by hydrogen and silica flour disproportionation in a fluidized bed reactor by plasma heating and prepare trichlorosilane, its Synchronous Heating through vaporization silicon tetrachloride and hydrogen make-up mixed gas, reduce heat-exchange equipment, reduce equipment failure; Improve the thermograde in fluidized-bed reactor, make in fluidized-bed reactor, to obtain thermal field even; Hydrogen plasma is provided, significantly improves converting silicon tetrachloride rate, reduce energy consumption.
To disclosed above-mentioned explanation, professional and technical personnel in the field are realized or uses the utility model.
To be apparent for those skilled in the art to the multiple amendment of these above-mentioned explanations, General Principle as defined herein when not departing from spirit or scope of the present utility model, can realize in other embodiments.Therefore, the utility model can not be restricted to above-mentioned explanation shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (2)
1. the device of trichlorosilane prepared by a plasma heating fluidized-bed, it is characterized in that: described device comprises: fluidized-bed reactor (10), hot water radiation wire (8) is provided with in fluidized-bed reactor (10), fluidized-bed reactor (10) wall is provided with silica flour charging opening (11), measurement and control of temperature mouth (12) and pressure warning unit (9), fluidized-bed reactor (10) bottom is provided with plasma gun (3) and hydrogen and silicon tetrachloride gas mixer (6), plasma gun (3) is connected with plasma heat source body (2), plasma heat source body (2) is connected with plasma power supply working gas entrance (1), hydrogen is connected with vaporizer (14) with hydrogen inlet (4) with silicon tetrachloride gas mixer (6), vaporizer (14) is provided with silicon tetrachloride entrance (5), heating agent entrance (15) and heating agent outlet (16), fluidized-bed reactor (10) top is provided with offgas outlet (13).
2. the device of trichlorosilane prepared by a kind of plasma heating fluidized-bed according to claim 1, it is characterized in that: described fluidized-bed reactor (10) is outside equipped with thermal insulation layer (7).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420589670.7U CN204138354U (en) | 2014-10-14 | 2014-10-14 | The device of trichlorosilane prepared by plasma heating fluidized-bed |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420589670.7U CN204138354U (en) | 2014-10-14 | 2014-10-14 | The device of trichlorosilane prepared by plasma heating fluidized-bed |
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| Publication Number | Publication Date |
|---|---|
| CN204138354U true CN204138354U (en) | 2015-02-04 |
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|---|---|---|---|
| CN201420589670.7U Expired - Fee Related CN204138354U (en) | 2014-10-14 | 2014-10-14 | The device of trichlorosilane prepared by plasma heating fluidized-bed |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107673358A (en) * | 2016-08-01 | 2018-02-09 | 新特能源股份有限公司 | A kind of cold hydrogenation prepares the system and method for trichlorosilane |
-
2014
- 2014-10-14 CN CN201420589670.7U patent/CN204138354U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107673358A (en) * | 2016-08-01 | 2018-02-09 | 新特能源股份有限公司 | A kind of cold hydrogenation prepares the system and method for trichlorosilane |
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| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150204 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |