CN201850145U - Reactor for producing trichlorosilane - Google Patents
Reactor for producing trichlorosilane Download PDFInfo
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- CN201850145U CN201850145U CN2010205255428U CN201020525542U CN201850145U CN 201850145 U CN201850145 U CN 201850145U CN 2010205255428 U CN2010205255428 U CN 2010205255428U CN 201020525542 U CN201020525542 U CN 201020525542U CN 201850145 U CN201850145 U CN 201850145U
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- opening
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Abstract
The utility model provides a reactor for producing trichlorosilane, which is characterized in that the reactor comprises a tubular body, a first baffle plate and a second baffle plate which are arranged on the tubular body at intervals along the axial direction of the tubular body, wherein a first opening, a second opening, a third opening and a fourth opening are formed on the tubular body, the second opening and the third opening are positioned between the second opening and the fourth opening, the first baffle plate is arranged between the first opening and the second opening, the second baffle plate is arranged between the second opening and the third opening, and the first baffle plate and the second baffle plate are air permeable orifice plates. The reactor provided by the utility model can ensure that silicon and silicon tetrachloride are conveyed into different reaction areas, and respectively control the reaction depth of each reaction area, and can obtain the high-yield and high-quality trichlorosilane products without increasing the quantity of the catalyst.
Description
Technical field
The utility model relates to a kind of reactor of producing trichlorosilane.
Background technology
At present, the improvement Siemens Method is the main flow technology of producing polysilicon both at home and abroad.Silicon tetrachloride and hydrogenchloride are the main byproducts that this explained hereafter polysilicon produces.1 ton of polysilicon of every production can produce silicon tetrachloride and the about 1-5 ton hydrogenchloride more than 10 tons.Because the SiCl that also not have extensive, high-level efficiency and produced in the digestion process production polysilicon process safely
4Method, caused hoarding of a large amount of high-content chlorine compounds, brought great hidden danger to environmental safety.
In recent years, the hydrogenation of silicon tetrachloride technology begins to obtain more and more personages' approval as an effective way that effectively solves polysilicon industry by-product, pollution problem, realization polysilicon industry sealing and circulating.
External polysilicon station-service hydride process processing of SiC l
4Technology, wherein a kind of technological line is SiCl
4Hot hydrogenation is about to SiCl
4And H
2Under 1200 ℃-1500 ℃ and 0.6MPa pressure, be converted into SiHCl
3Chemical equation is: SiCl
4+ H
2→ SiHCl
3+ HCl.But this method temperature of reaction height, energy consumption is big, and one time transformation efficiency is low, is up to 18%.
Another kind of technological line is SiCl
4Cold hydrogenation.Generally be with diatomite, gac, Al
2O
3For granular nickel salt, the mantoquita of carrier is catalyzer, control certain temperature, pressure, make H
2With SiCl
4Mixed gas and silica flour contact with boiling state in reactor and carry out hydrogenation, part of SiC l
4Change into SiHCl
3, the SiCl in its product
4Its conversion that circulates is repeatedly reclaimed.For example, CN1436725A discloses the cold method for hydrogenation that a kind of hydrogenation of silicon tetrachloride is produced trichlorosilane, wherein silica flour, SiCl
4And H
2Trichlorosilane is produced in reaction in the ebullated bed reactor of inner bag heating.
Another method is the chlorine hydrogenation of silicon tetrachloride, and wherein silicon tetrachloride, hydrogen, hydrogenchloride and metalluragical silicon carry out gas solid catalytic reaction in fluidized-bed, generates the gas phase trichlorosilane.The trichlorosilane that transforms can be used for production of polysilicon, thereby has improved the utilization ratio of raw materials that is used to produce polysilicon, has reduced manufacturing cost.CN20113671Y discloses a kind of chlorine hydride process that utilizes silicon tetrachloride has been converted into the device of trichlorosilane, utilizes silica flour, SiCl
4, HCl and H
2Trichlorosilane is produced in reaction in ebullated bed reactor.Yet, adopt above-mentioned reactor to produce trichlorosilane and have the lower problem of silicon tetrachloride transformation efficiency.
Therefore, need improve,, reduce material consumption, energy consumption to enhance productivity to reactor and the method for utilizing polysilicon by-product production trichlorosilane.
The utility model content
The purpose of this utility model is to produce SiHCl in order to overcome pre-existing reactors
3There is SiCl
4The shortcoming that transformation efficiency is low provides the high hydrogenation of silicon tetrachloride that utilizes of a kind of silicon tetrachloride transformation efficiency to produce the reactor of trichlorosilane.
Contriver of the present utility model finds that there is SiCl in prior art
4The reason that transformation efficiency is low may be, in the above-mentioned existing hydrogenation technique, carrying out a plurality of reactions simultaneously, and its principal reaction comprises:
Si+3HCl(g)=H
2(g)+SiHCl
3(g) (1)
SiCl
4(g)+H
2(g)=SiHCl
3(g)+HCl(g) (2)
Si+3SiCl
4(g)+2H
2(g)=4SiHCl
3(g) (3)
Thermomechanical analysis is the result show, above-mentioned optimum reaction conditions is different.From these equilibrium constant of reaction, it is unfavorable to the reaction (1) of Si and HCl to improve temperature; And SiCl
4(g)+H
2(g) reaction (2) is thermo-negative reaction, so it is favourable to reaction (2) to improve temperature; This just makes Si+3SiCl
4(g)+2H
2(g) reaction (3) must be carried out under appropriate reaction conditions, all obtains preferable transformation efficiency to satisfy two kinds of reactions simultaneously.
But clearly, SiCl
4Hydrogenation prepares SiHCl
3With Si and HCl prepared in reaction SiHCl
3Influence each self-reacting optimization in same reaction zone reaction, for example, (1) catalyzer mixes with a large amount of silica flours, makes catalyzer disperse, and causes in order to obtain higher transformation efficiency, and catalyst levels is bigger; (2) influence SiCl
4The optimization of charging air speed; (3) can't adopt and satisfy each self-reacting optimum catalyst, the copper catalyst that is more suitable for reaction (2) caking easily under existence conditions, influence is active.
The utility model provides a kind of reactor of producing trichlorosilane, it is characterized in that, this reactor comprises cylindrical body and is arranged on first dividing plate and second partition in this cylindrical body along the axially spaced-apart of this cylindrical body, offer first opening on the described cylindrical body, second opening, the 3rd opening and the 4th opening, second opening and the 3rd opening are between first opening and the 4th opening, described first dividing plate is arranged between first opening and second opening, described second partition is arranged between second opening and the 3rd opening, and described first dividing plate and second partition are the ventilation property orifice plate.
The reactor that the utility model provides can realize making silicon to enter different reaction zones respectively with silicon tetrachloride, and controls the reaction depth of each reaction zone respectively, thereby obtains high yield, high-quality trichlorosilane product.Adopt reactor of the present utility model can make the transformation efficiency of silicon tetrachloride reach 30.1%, and use the reactor of prior art, the transformation efficiency of silicon tetrachloride only is 18%.
Description of drawings
A kind of structural representation of the reactor of the production trichlorosilane that Fig. 1 provides for the utility model.
The another kind of structural representation of the reactor of the production trichlorosilane that Fig. 2 provides for the utility model.
Embodiment
The reactor of the production trichlorosilane that the utility model is provided below in conjunction with accompanying drawing is elaborated.
The reactor of the production trichlorosilane that the utility model provides as depicted in figs. 1 and 2, it is characterized in that, this reactor comprises cylindrical body and is arranged on first dividing plate and second partition in this cylindrical body along the axially spaced-apart of this cylindrical body, offer the first opening a, the second opening b, the 3rd opening c and the 4th opening d on the described cylindrical body, the second opening b and the 3rd opening c are between the first opening a and the 4th opening d, described first dividing plate is arranged between the first opening a and the second opening b, described second partition g
2Be arranged between the second opening b and the 3rd opening c the described first dividing plate g
1With second partition g
2Be the ventilation property orifice plate.
According to the utility model, described the 4th opening d is positioned at the top of described cylindrical body, the described first dividing plate g
1With second partition g
2Between distance A and described second partition g
2And can in a big way, change between the 4th opening d apart from the ratio between the B, preferably, the described first dividing plate g
1With second partition g
2Between distance A and described second partition g
2And satisfy A apart from B between the 4th opening d: B=1: 2-10.
According to the utility model, the described second opening b and the first dividing plate g
1Between distance C and the described first dividing plate g
1With second partition g
2Between the ratio of distance D can in a big way, change, preferably, the described second opening b and the first dividing plate g
1Between distance C and the described first dividing plate g
1With second partition g
2Between distance D satisfy D: E=1: 0.1-0.5.
According to the utility model, described the 3rd opening c and second partition g
2Between apart from E and described second partition g
2And can in a big way, change between the 4th opening d apart from the ratio between the F, preferably, described the 3rd opening c and second partition g
2Between apart from E and described second partition g
2And satisfy E apart from F between the 4th opening d: F=1: 0.1-0.3.
According to the utility model, the described first dividing plate g
1With described second partition g
2All can be the ventilation property orifice plate, described ventilation property orifice plate can for any can penetrating gas and hold back solid particulate such as the orifice plate of silica flour and granules of catalyst, as gas distributor, gas distributor can make the gas that enters this reaction zone mix more even, help the raising of reaction efficiency, dividing plate is preferably gas distributor described in the utility model.
According to the utility model, the described first dividing plate g
1With described second partition g
2Bore dia can be 0.5-3mm, the described first dividing plate g
1The total area in hole can be the 20-60% of this dividing plate area, described second partition g
2The total area in hole can be the 20-60% of this dividing plate area.By making the first dividing plate g
1With second partition g
2Bore dia in above-mentioned scope, can in use make the gas silicon tetrachloride by holding back granules of catalyst and silicon powder particle; By making the first dividing plate g
1With second partition g
2The total area in hole in above-mentioned scope, can make gas smoothly by dividing plate and be evenly distributed in the cylindrical body of outlet side of dividing plate and react.
According to the utility model, can also be provided with screen cloth in the cylindrical body between described the 3rd opening c and the 4th opening d, the bore dia of described screen cloth can be the 10-30 micron.
According to the utility model, described cylindrical body can be divided into two parts, comprises the first barrel I and the second barrel II, and the described first barrel I is the first dividing plate g
1With second partition g
2Between part, this part forms first reaction zone, the described second barrel II is second partition g
2And the part between the 3rd opening c, this part forms second reaction zone.Under the preferable case, the cross-sectional area ratio of the first barrel I and the second barrel II is 1: 0.2-1, the promptly described first barrel I and the second barrel II can isometrical (as shown in Figure 2), also can reducing (as shown in Figure 1).When first reaction zone and second reaction zone during all as fixed-bed reactor, the preferred first barrel I and the second barrel II are isometrical; When first reaction zone and second reaction zone during respectively as fixed-bed reactor and fluidized-bed reactor, the preferred described first barrel I and the second barrel II are reducing, and the diameter of the described first barrel I is greater than the diameter of the second barrel II, and more preferably the cross-sectional area ratio of the first barrel I and the second barrel II is 1: 0.2-0.9.
According to the utility model, the described first barrel I and the second barrel II can have any shape, the cross-sectional area of the described first barrel I and the second barrel II is the area in cross section, optional position, under the preferable case, the described first barrel I and the second barrel II are cylindrical tube shape.
According to the utility model, this reactor can also comprise the 3rd barrel III, described the 3rd barrel III is the part between the 3rd opening c and the 4th opening d, be used for carrying out settlement separate to reaction product from second reaction zone, isolated gas is discharged by the 4th opening d, solid then can return second reaction zone or discharge, and described the 3rd barrel III is 2-6 with the cross-sectional area ratio of the second barrel II: 1.
According to the utility model, this reactor can also comprise refrigerating unit, refrigerating unit can reduce temperature and reclaim heat, and realizing total energy approach, described refrigerating unit is arranged on the outside of the cylindrical body between the described second opening b and the 3rd opening c or inner.
According to the utility model, this refrigerating unit can be various forms of refrigerating units, for example, can be for stretching into the interchanger of cylindrical body inside, under the preferable case, this refrigerating unit comprises housing, this housing and described second partition g
2And the 3rd cylindrical body between the opening c form cavity, this cavity is in communication with the outside by the 5th opening e and the 6th opening f.During use, heat-eliminating medium can feed from the 5th opening e or the 6th opening f, flow out from the 6th opening f or the 5th opening e, by heat-eliminating medium to lowering the temperature in the cylindrical body.
Below in conjunction with accompanying drawing 1, introduce a kind of method that the reactor utilize the production trichlorosilane that the utility model provides realizes producing trichlorosilane.
This method comprises passes through the first opening a and the first dividing plate g with silicon tetrachloride and hydrogen
1Enter first reaction zone, be provided with the beds that forms by catalyzer and silica flour in first reaction zone, described catalyzer and silica flour join in first reaction zone by the second opening b, silicon tetrachloride contacts in first reaction zone with silica flour with nickel-base catalyst with hydrogen, is mainly contained first gaseous mixture of trichlorosilane, silicon tetrachloride and hydrogenchloride; This first gaseous mixture is by second partition g
2Enter second reaction zone, the second reaction zone cylindrical body outer cover is provided with a housing as refrigerating unit, feed thermal oil in this housing as heat-eliminating medium, thermal oil enters housing from the 5th opening e, leave housing from the 6th opening f, realize the exchange of heat, make the temperature of first gaseous mixture drop to optimal temperature, to contact with silica flour, described silica flour joins in second reaction zone by the 3rd opening c, and reaction is mainly contained second gaseous mixture of trichlorosilane and silicon tetrachloride, and this second gaseous mixture leaves reactor by the 4th opening d, separate this second gaseous mixture, obtain the trichlorosilane product.
Claims (10)
1. reactor of producing trichlorosilane, it is characterized in that, this reactor comprises cylindrical body and is arranged on first dividing plate and second partition in this cylindrical body along the axially spaced-apart of this cylindrical body, offer first opening on the described cylindrical body, second opening, the 3rd opening and the 4th opening, second opening and the 3rd opening are between first opening and the 4th opening, described first dividing plate is arranged between first opening and second opening, described second partition is arranged between second opening and the 3rd opening, and described first dividing plate and second partition are the ventilation property orifice plate.
2. reactor according to claim 1, it is characterized in that, described the 4th opening is positioned at the top of described cylindrical body, satisfies A apart from B between distance A between described first dividing plate and the second partition and described second partition and the 4th opening: B=1: 2-10.
3. reactor according to claim 2 is characterized in that, the distance D between the distance C between described second opening and first dividing plate and described first dividing plate and the second partition satisfies C: D=1: 0.1-0.5.
4. reactor according to claim 2 is characterized in that, between described the 3rd opening and the second partition apart from satisfying E apart from F between E and described second partition and the 4th opening: F=1: 0.1-0.3.
5. reactor according to claim 1, it is characterized in that, the bore dia of described first dividing plate and described second partition is 0.5-3mm, and the total area in the hole of described first dividing plate is the 20-60% of this dividing plate area, and the total area in the hole of described second partition is the 20-60% of this dividing plate area.
6. according to any described reactor among the claim 1-5, it is characterized in that also be provided with screen cloth in the cylindrical body between described the 3rd opening and the 4th opening, the bore dia of described screen cloth is the 10-30 micron.
7. according to any described reactor among the claim 1-5, it is characterized in that, described cylindrical body comprises first barrel and second barrel, described first barrel is the part between first dividing plate and the second partition, described second barrel is the part between second partition and the 3rd opening, and the cross-sectional area ratio of first barrel and second barrel is 1: 0.2-1.
8. reactor according to claim 7, it is characterized in that, described cylindrical body also comprises the 3rd barrel, and described the 3rd barrel is the part between the 3rd opening and the 4th opening, and the 3rd barrel is 2-6 with the cross-sectional area ratio of second barrel: 1.
9. reactor according to claim 7 is characterized in that this reactor also comprises refrigerating unit, and described refrigerating unit is arranged on the outside or inner of cylindrical body between described second opening and the 3rd opening.
10. reactor according to claim 9 is characterized in that this refrigerating unit comprises housing, and the cylindrical body between this housing and described second partition and the 3rd opening forms cavity, and this cavity is in communication with the outside by the 5th opening and the 6th opening.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2010205255428U CN201850145U (en) | 2010-09-08 | 2010-09-08 | Reactor for producing trichlorosilane |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2010205255428U CN201850145U (en) | 2010-09-08 | 2010-09-08 | Reactor for producing trichlorosilane |
Publications (1)
Publication Number | Publication Date |
---|---|
CN201850145U true CN201850145U (en) | 2011-06-01 |
Family
ID=44092547
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN2010205255428U Expired - Fee Related CN201850145U (en) | 2010-09-08 | 2010-09-08 | Reactor for producing trichlorosilane |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN201850145U (en) |
-
2010
- 2010-09-08 CN CN2010205255428U patent/CN201850145U/en not_active Expired - Fee Related
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Legal Events
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: 20110601 Termination date: 20140908 |
|
EXPY | Termination of patent right or utility model |