CN104140105A - Device for preparing trichlorosilane - Google Patents
Device for preparing trichlorosilane Download PDFInfo
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- CN104140105A CN104140105A CN201410345651.4A CN201410345651A CN104140105A CN 104140105 A CN104140105 A CN 104140105A CN 201410345651 A CN201410345651 A CN 201410345651A CN 104140105 A CN104140105 A CN 104140105A
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Abstract
The invention discloses a device for preparing trichlorosilane. The device comprises a rectifying tower body, a silicon tetrachloride inlet, a dichlorosilane inlet, a heavy component outlet, a light component outlet, a trichlorosilane outlet, a reboiler and a condenser. A rectifying area, a reacting area and a distilling area are sequentially defined in the rectifying tower body from top to bottom. The silicon tetrachloride inlet is formed between the distilling area and the reacting area. The dichlorosilane inlet is formed between the reacting area and the distilling area. The heavy component outlet is formed in the bottom of the distilling area. The trichlorosilane outlet is formed in the top of the distilling area. The reboiler is provided with a liquid inlet and a gas outlet, the liquid inlet is connected with the heavy component outlet, and the gas outlet is connected with the distilling area. The condenser is provided with a gaseous state light component inlet, a reflux outlet and a trichlorosilane outlet. The gaseous state light component inlet is connected with the light component outlet, and the reflux outlet is connected with the rectifying area. The device can solve the problems that dichlorosilane cannot be processed in a large scale, and the converting rate of the dichlorosilane is low.
Description
Technical field
The invention belongs to technical field of polysilicon production, particularly, the present invention relates to a kind of device of preparing trichlorosilane.
Background technology
Produce in the technique of polysilicon at improved Siemens, have a small amount of by product dichloro-dihydro silicon and be separated in rectifying workshop section.Although also reacting as raw material in reduction furnace, dichloro-dihydro silicon generates polysilicon, but need independent a set of reduction system, and the amount of dichloro-dihydro silicon is little, and has more amorphous silicon generation, effect is not very desirable, and a lot of enterprises directly sell dichloro-dihydro silicon.
Along with the expansion of production of polysilicon scale, the amount of dichloro-dihydro silicon also more gets up, dichloro-dihydro silicon is a kind of inflammable, explosive hazardous chemical, and storage and transport have all brought very large burden to enterprise, needs a kind of method of better processing dichloro-dihydro silicon to process dichloro-dihydro silicon.
Therefore, the technology of existing processing dichloro-dihydro silicon needs further to be studied.
Summary of the invention
The present invention is intended to solve at least to a certain extent one of technical problem in correlation technique.For this reason, one object of the present invention is to propose a kind of device of preparing trichlorosilane, and this device can solve a difficult problem and the low problem of dichloro-dihydro silicon conversion that dichloro-dihydro silicon cannot be processed on a large scale.
In one aspect of the invention, the present invention proposes a kind of device of preparing trichlorosilane, this device comprises:
Rectifying tower body, limits rectification zone, reaction zone and distillation zone from top to bottom successively in described rectifying tower body;
Silicon tetrachloride entrance, described silicon tetrachloride entrance is arranged between described rectification zone and described reaction zone;
Dichloro-dihydro silicon entrance, described dichloro-dihydro silicon entrance is arranged between described reaction zone and described distillation zone;
Heavy constituent outlet, described heavy constituent outlet is arranged on the bottom of described distillation zone;
Light constituent outlet, described light constituent outlet is arranged on the top of described rectification zone;
Reboiler, described reboiler has liquid inlet and pneumatic outlet, and described liquid inlet is connected with the outlet of described heavy constituent, and described pneumatic outlet is connected with described distillation zone; And
Condenser, described condenser has gaseous light component entrance, phegma outlet and trichlorosilane outlet, and described gaseous light component entrance is connected with described light constituent outlet, and described phegma outlet is connected with described rectification zone.
Pass through distiller according to the device of preparing trichlorosilane of the embodiment of the present invention, reactor and rectifying tower are incorporated into Dan Tazhong, a difficult problem and the low problem of dichloro-dihydro silicon conversion that dichloro-dihydro silicon cannot be processed are on a large scale solved, and a large amount of dichloro-dihydro silicon is converted into the trichlorosilane (purity is greater than 99%) of high added value, simultaneously by integrating, obviously having saved facility investment and equipment takes up an area, thereby save processing cost, in addition, this device operating pressure and operating temperature are all lower, heat-eliminating medium used is recirculated water, thermal source is water vapour, make device safe and reliable in operational process, and this device does not have exhaust emissions, thereby reach the object of environmental protection.
In addition, the device of preparing trichlorosilane according to the above embodiment of the present invention can also have following additional technical characterictic:
In some embodiments of the invention, described rectification zone and described distillation zone internals are sieve plate respectively independently.Thus, can significantly improve the purity of trichlorosilane.
In some embodiments of the invention, the theoretical plate number of described rectification zone is 15～18.Thus, can further improve the purity of trichlorosilane.
In some embodiments of the invention, the theoretical plate number of described distillation zone is 5～8.Thus, can significantly improve distillation processing efficiency.
In some embodiments of the invention, described reaction zone comprises catalyst layer.Thus, can significantly improve the transformation efficiency of dichloro-dihydro silicon.
In some embodiments of the invention, described catalyst layer is higher than 2 meters.Thus, can further improve the transformation efficiency of dichloro-dihydro silicon.
Brief description of the drawings
Fig. 1 is the apparatus structure schematic diagram of preparing according to an embodiment of the invention trichlorosilane.
Embodiment
Describe embodiments of the invention below in detail, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has the element of identical or similar functions from start to finish.Be exemplary below by the embodiment being described with reference to the drawings, be intended to for explaining the present invention, and can not be interpreted as limitation of the present invention.
In description of the invention, it will be appreciated that, term " " center ", " longitudinally ", " laterally ", " length ", " width ", " thickness ", " on ", D score, " front ", " afterwards ", " left side ", " right side ", " vertically ", " level ", " top ", " end " " interior ", " outward ", " clockwise ", " counterclockwise ", " axially ", " radially ", orientation or the position relationship of instructions such as " circumferentially " are based on orientation shown in the drawings or position relationship, only the present invention for convenience of description and simplified characterization, instead of device or the element of instruction or hint indication must have specific orientation, with specific orientation structure and operation, therefore can not be interpreted as limitation of the present invention.
In the present invention, unless otherwise clearly defined and limited, the terms such as term " installation ", " being connected ", " connection ", " fixing " should be interpreted broadly, and for example, can be to be fixedly connected with, and can be also to removably connect, or integral; Can be mechanical connection, can be also electrical connection; Can be to be directly connected, also can indirectly be connected by intermediary, can be the connection of two element internals or the interaction relationship of two elements, unless separately there is clear and definite restriction.For the ordinary skill in the art, can understand as the case may be above-mentioned term concrete meaning in the present invention.
In the present invention, unless otherwise clearly defined and limited, First Characteristic Second Characteristic " on " or D score can be that the first and second features directly contact, or the first and second features are by intermediary indirect contact.And, First Characteristic Second Characteristic " on ", " top " and " above " but First Characteristic directly over Second Characteristic or oblique upper, or only represent that First Characteristic level height is higher than Second Characteristic.First Characteristic Second Characteristic " under ", " below " and " below " can be First Characteristic under Second Characteristic or tiltedly, or only represent that First Characteristic level height is less than Second Characteristic.
In one aspect of the invention, the present invention proposes a kind of device of preparing trichlorosilane.Below with reference to Fig. 1, the device of preparing trichlorosilane of the embodiment of the present invention is described in detail.According to an embodiment of the invention, this device comprises:
Rectifying tower body 100: according to embodiments of the invention, limit rectification zone 11, reaction zone 12 and distillation zone 13 with this from top to bottom in rectifying tower body.According to embodiments of the invention, between reaction zone 12 and distillation zone 13, be provided with silicon tetrachloride entrance 14, for silicon tetrachloride being supplied to rectifying tower body 100.According to embodiments of the invention, between rectification zone 11 and reaction zone 12, be provided with dichloro-dihydro silicon entrance 15, for dichloro-dihydro silicon is supplied to rectifying tower body 100.According to embodiments of the invention, the bottom of distillation zone 13 is provided with heavy constituent outlet 16, discharges rectifying tower body 100 for the heavy constituent that process is produced.According to embodiments of the invention, the top of rectification zone 11 is provided with light constituent outlet 17, discharges rectifying tower body 100 for the light constituent that process is produced.
According to embodiments of the invention, the charging of dichloro-dihydro silicon is also not particularly limited, and according to a particular embodiment of the invention, the feeding rate of dichloro-dihydro silicon can be 13kmol/h.According to embodiments of the invention, the raw materials components mole ratio of dichloro-dihydro silicon and silicon tetrachloride can be 0.9～1:1.Contriver's discovery, this raw materials components mole ratio can significantly improve the transformation efficiency of dichloro-dihydro silicon.According to embodiments of the invention, the treatment condition of rectification zone are also not particularly limited, and according to a particular embodiment of the invention, the temperature of rectification zone can be 90～97 degrees Celsius, and pressure can be 0.1～0.6MPa.According to embodiments of the invention, the internals of rectification zone can be sieve plate, and the theoretical plate number of rectification zone can be 15～18.According to embodiments of the invention, the theoretical plate number of distillation zone can be 5～8.According to embodiments of the invention, reaction zone can comprise catalyst layer, and the height of catalyst layer is higher than 2 meters.According to embodiments of the invention, the concrete kind of catalyzer is also not particularly limited, and according to a particular embodiment of the invention, catalyzer can be ion exchange resin.Thus, can further improve the transformation efficiency of dichloro-dihydro silicon.
Reboiler 200: according to embodiments of the invention, reboiler 200 has liquid inlet 21 and pneumatic outlet 22, and liquid inlet 21 is connected with heavy constituent outlet 16, pneumatic outlet 22 is connected with distillation zone 13, for the heavy constituent obtaining is carried out to heat treated, thereby provide heat for rectifying tower body.According to embodiments of the invention, heavy constituent can contain silicon tetrachloride.
Condenser 300: according to embodiments of the invention, condenser 300 has gaseous light component entrance 31, phegma outlet 32 and trichlorosilane outlet 33, and gaseous light component entrance 31 is connected with light constituent outlet 17, phegma outlet 32 is connected with rectification zone 11, and carry out condensation process for the light constituent that rectifying tower body is produced, thereby obtain liquid light constituent, and a part for obtained liquid light constituent is back to rectification zone as phegma.According to embodiments of the invention, light constituent can contain trichlorosilane.According to embodiments of the invention, the liquid light constituent that returns to rectification zone can be 13.5～18.5 with the ratio of obtained gaseous light component.
Concrete, silicon tetrachloride and dichloro-dihydro silicon are supplied in rectifying tower body from silicon tetrachloride entrance and dichloro-dihydro silicon entrance respectively, silicon tetrachloride enters distillation zone from top to bottom, then in reboiler, be heated as silicon tetrachloride vapor through water vapour, thereby dichloro-dihydro silicon runs into the silicon tetrachloride vapor of coming from reboiler and becomes gas from bottom to top through reaction zone, silicon tetrachloride contacts at the catalyzer place of reaction zone with dichloro-dihydro silicon anti-disproportionation reaction generation trichlorosilane occurs, contain unreacted silicon tetrachloride heavy constituent and continue to drop to distillation zone through heavy constituent outlet discharge rectifying tower body, and a part for obtained heavy constituent is become to steam after reboiler provide heat for rectifying tower body, what reaction zone obtained contains trichlorosilane, a small amount of silicon tetrachloride and micro-dichloro-dihydro silicon mixture rising enter rectification zone and carry out rectification process, the light constituent that contains gaseous state trichlorosilane obtaining is discharged rectifying tower body through light constituent outlet, enter condenser and carry out condensation process, obtain liquid trichlorosilane, and be back to rectification zone using a part for liquid trichlorosilane as phegma and proceed rectification process, and continuing to drop to reaction zone, the heavy constituent that rectification zone obtains containing silicon tetrachloride carries out anti-disproportionation reaction.
Pass through distiller according to the device of preparing trichlorosilane of the embodiment of the present invention, reactor and rectifying tower are incorporated into Dan Tazhong, a difficult problem and the low problem of dichloro-dihydro silicon conversion that dichloro-dihydro silicon cannot be processed are on a large scale solved, and a large amount of dichloro-dihydro silicon is converted into the trichlorosilane (purity is greater than 99%) of high added value, simultaneously by integrating, obviously having saved facility investment and equipment takes up an area, thereby save processing cost, in addition, this device operating pressure and operating temperature are all lower, heat-eliminating medium used is recirculated water, thermal source is water vapour, make device safe and reliable in operational process, and this device does not have exhaust emissions, thereby reach the object of environmental protection.
Understand for convenient, the method that the device of preparing trichlorosilane below to utilizing is prepared trichlorosilane is described in detail.According to embodiments of the invention, the method comprises: silicon tetrachloride and dichloro-dihydro silicon are supplied in rectifying tower body from silicon tetrachloride entrance and the dichloro-dihydro silicon entrance of the above-mentioned device of preparing trichlorosilane respectively; Make the intrinsic silicon tetrachloride of rectifying tower change into silicon tetrachloride vapor after reboiler heating and enter reaction zone; Make silicon tetrachloride vapor and dichloro-dihydro silicon that anti-disproportionation reaction occur in described reaction zone, to obtain the mixture that contains trichlorosilane, dichloro-dihydro silicon and silicon tetrachloride; The mixture that contains trichlorosilane, dichloro-dihydro silicon and silicon tetrachloride is carried out in rectification zone to rectification process, obtain gaseous state trichlorosilane to separate; And gaseous state trichlorosilane is carried out in condenser to condensation process, to obtain liquid trichlorosilane, and a part for liquid trichlorosilane is back to described rectification zone.
According to embodiments of the invention, the charging of dichloro-dihydro silicon is also not particularly limited, and according to a particular embodiment of the invention, the feeding rate of dichloro-dihydro silicon can be 13kmol/h.According to embodiments of the invention, the raw materials components mole ratio of dichloro-dihydro silicon and silicon tetrachloride can be 0.9～1:1.Contriver's discovery, this raw materials components mole ratio can significantly improve the transformation efficiency of dichloro-dihydro silicon.According to embodiments of the invention, the treatment condition of rectification zone are also not particularly limited, and according to a particular embodiment of the invention, the temperature of rectification zone can be 90～97 degrees Celsius, and pressure can be 0.1～0.6MPa.According to embodiments of the invention, the internals of rectification zone can be sieve plate, and the theoretical plate number of rectification zone can be 15～18.According to embodiments of the invention, the theoretical plate number of distillation zone can be 5～8.According to embodiments of the invention, reaction zone can comprise catalyst layer, and the height of catalyst layer is higher than 2 meters.According to embodiments of the invention, the concrete kind of catalyzer is also not particularly limited, and according to a particular embodiment of the invention, catalyzer can be ion exchange resin.Thus, can further improve the transformation efficiency of dichloro-dihydro silicon.
Utilize method that the device of preparing trichlorosilane of the embodiment of the present invention prepares trichlorosilane by distilling, anti-disproportionation reaction and rectification process are incorporated into Dan Tazhong and carry out, a difficult problem and the low problem of dichloro-dihydro silicon conversion that dichloro-dihydro silicon cannot be processed are on a large scale solved, and a large amount of dichloro-dihydro silicon is converted into the trichlorosilane (purity is greater than 99%) of high added value, simultaneously by integrating, obviously having saved facility investment and equipment takes up an area, thereby save processing cost, in addition, this device operating pressure and operating temperature are all lower, heat-eliminating medium used is recirculated water, thermal source is water vapour, make device safe and reliable in operational process, and this device does not have exhaust emissions, thereby reach the object of environmental protection.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means to be contained at least one embodiment of the present invention or example in conjunction with specific features, structure, material or the feature of this embodiment or example description.In this manual, to the schematic statement of above-mentioned term not must for be identical embodiment or example.And, specific features, structure, material or the feature of description can one or more embodiment in office or example in suitable mode combination.In addition,, not conflicting in the situation that, those skilled in the art can carry out combination and combination by the feature of the different embodiment that describe in this specification sheets or example and different embodiment or example.
Although illustrated and described embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, and those of ordinary skill in the art can change above-described embodiment within the scope of the invention, amendment, replacement and modification.
Claims (6)
1. a device of preparing trichlorosilane, is characterized in that, comprising:
Rectifying tower body, limits rectification zone, reaction zone and distillation zone from top to bottom successively in described rectifying tower body;
Silicon tetrachloride entrance, described silicon tetrachloride entrance is arranged between described rectification zone and described reaction zone;
Dichloro-dihydro silicon entrance, described dichloro-dihydro silicon entrance is arranged between described reaction zone and described distillation zone;
Heavy constituent outlet, described heavy constituent outlet is arranged on the bottom of described distillation zone;
Light constituent outlet, described light constituent outlet is arranged on the top of described rectification zone;
Reboiler, described reboiler has liquid inlet and pneumatic outlet, and described liquid inlet is connected with the outlet of described heavy constituent, and described pneumatic outlet is connected with described distillation zone; And
Condenser, described condenser has gaseous light component entrance, phegma outlet and trichlorosilane outlet, and described gaseous light component entrance is connected with described light constituent outlet, and described phegma outlet is connected with described rectification zone.
2. the device of preparing trichlorosilane according to claim 1, is characterized in that, described rectification zone and described distillation zone internals are sieve plate respectively independently.
3. the device of preparing trichlorosilane according to claim 2, is characterized in that, the theoretical plate number of described rectification zone is 15～18.
4. the device of preparing trichlorosilane according to claim 2, is characterized in that, the theoretical plate number of described distillation zone is 5～8.
5. the device of preparing trichlorosilane according to claim 1, is characterized in that, described reaction zone comprises catalyst layer.
6. the device of preparing trichlorosilane according to claim 5, is characterized in that, described catalyst layer is higher than 2 meters.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410345651.4A CN104140105A (en) | 2014-07-18 | 2014-07-18 | Device for preparing trichlorosilane |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410345651.4A CN104140105A (en) | 2014-07-18 | 2014-07-18 | Device for preparing trichlorosilane |
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| CN104140105A true CN104140105A (en) | 2014-11-12 |
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| CN201410345651.4A Pending CN104140105A (en) | 2014-07-18 | 2014-07-18 | Device for preparing trichlorosilane |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113019265A (en) * | 2021-03-16 | 2021-06-25 | 中国恩菲工程技术有限公司 | Reaction device and method for preparing final product by using same |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103253676A (en) * | 2013-05-10 | 2013-08-21 | 河北工业大学 | Preparation method of trichlorosilane |
| CN103708471A (en) * | 2013-12-18 | 2014-04-09 | 天津大学 | Equipment and method for preparing chlorosilane from silane through reverse disproportionation |
| CN204039071U (en) * | 2014-07-18 | 2014-12-24 | 中国恩菲工程技术有限公司 | Prepare the device of trichlorosilane |
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- 2014-07-18 CN CN201410345651.4A patent/CN104140105A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103253676A (en) * | 2013-05-10 | 2013-08-21 | 河北工业大学 | Preparation method of trichlorosilane |
| CN103708471A (en) * | 2013-12-18 | 2014-04-09 | 天津大学 | Equipment and method for preparing chlorosilane from silane through reverse disproportionation |
| CN204039071U (en) * | 2014-07-18 | 2014-12-24 | 中国恩菲工程技术有限公司 | Prepare the device of trichlorosilane |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113019265A (en) * | 2021-03-16 | 2021-06-25 | 中国恩菲工程技术有限公司 | Reaction device and method for preparing final product by using same |
| CN113019265B (en) * | 2021-03-16 | 2022-09-20 | 中国恩菲工程技术有限公司 | Reaction device and method for preparing final product by using same |
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Application publication date: 20141112 |