CN102786055A - Method and device for heat utilization in polycrystalline silicon production process - Google Patents
Method and device for heat utilization in polycrystalline silicon production process Download PDFInfo
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- CN102786055A CN102786055A CN2012103205786A CN201210320578A CN102786055A CN 102786055 A CN102786055 A CN 102786055A CN 2012103205786 A CN2012103205786 A CN 2012103205786A CN 201210320578 A CN201210320578 A CN 201210320578A CN 102786055 A CN102786055 A CN 102786055A
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- hydrogenation reactor
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- chlorosilane
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Abstract
The invention provides a method and a device for heat utilization in a polycrystalline silicon production process. The method for heat utilization in the polycrystalline silicon production process comprises a synthetizing step of heating hydrogen and silicon tetrachloride generated in the polycrystalline silicon production process, introducing into a hydrogenation reactor carried with silicon powders, and carrying out hydrogenation to obtain mixed gas including trichlorosilane generated in the reaction; a purifying step of removing the silicon powder from the mixed gas by chlorosilane so as to obtain the purified gas including chlorosilan; a condensing step of introducing the purified gas in a re-boiler which is arranged on the bottom of a refining tower, exchanging heat and cooling, introducing the cooled condensed gas in a condenser, and condensing, so as to obtain condensed liquid and uncondensed gas; returning the uncondensed gas back to the hydrogenation reactor and feeding the condensed liquid in the refining tower; a refining step of using the gas separated from the top part of the refining tower as the raw material of a polycrystalline silicon reducing tower; and returning the liquid separated out from the kettle of the refining tower back to the hydrogenation reactor. According to the invention, the energy consumption in the polycrystalline silicon production process is reduced so that the production cost is reduced.
Description
Technical field
The present invention relates to field of polysilicon production, the device and method of Btu utilization in particularly a kind of polysilicon production process.
Background technology
The polysilicon preparation is the industry of a highly energy-consuming, and it is the emphasis of each Sustainable Development of Enterprises that improvement technology reduces production costs.Silicon tetrachloride (the SiCl that in polysilicon production process, produces
4) amount very big (according to data, every production 1kg polysilicon approximately will produce 22kg SiCl
4), for this reason, all explore both at home and abroad and effectively utilize SiCl in effort
4Desirable approach.Wherein, cold hydride process is processing of SiC l
4A kind of extremely effective means.The Production Flow Chart of the cold hydrogenation process routine of present domestic polysilicon is as shown in Figure 1, hydrogen (H
2) and SiCl
4Get into hydrogenation reactor after mixing post-heating to 600 ℃, reacting with silica flour in the hydrogenation reactor generates trichlorosilane (SiHCl
3), comprise SiHCl from what hydrogenation reactor came out
3With unreacted SiCl
4, H
2, silica flour and reaction by-product dichloro-dihydro silicon (SiH
2Cl
2), the mixed gas of hydrogenchloride (HCl) gets in the washing tower, sends into condensing surface after with chlorosilane the silica flour in the mixed gas being removed, through condensing surface with the SiHCl in the mixed gas
3, SiCl
4, SiH
2Cl
2Be condensed into chlorosilane liquid, send into rectifying tower then.The H that is not condensed
2Sending hydrogenation reactor back to HCl recycles.Outer supply steam and chlorosilane heat exchange in the rectifying tower tower bottom reboiler, chlorosilane is partly vaporized after the heat exchange, and is transported in the distillation tower as thermal source, and vapor phase becomes phlegma discharge reboiler.Rectifying obtains SiHCl in rectifying tower
3And SiCl
4, send into production of polysilicon system and hydrogenation reactor respectively and recycle.
In the cold hydrogenation process of existing polysilicon, have following defective at least: waste heat is not fully utilized, and energy consumption is big; Material does not fully rationally utilize, and causes waste.
Summary of the invention
The objective of the invention is to provides the device and method of Btu utilization in a kind of polysilicon production process to one of above-mentioned defective that exists in the prior art, reduces the energy consumption in production of polysilicon, reduces production costs.
According to an aspect of the present invention, the method for Btu utilization in a kind of polysilicon production process is provided, has comprised:
Synthesis step: with being incorporated in the hydrogenation reactor that is loaded with silica flour after hydrogen and the heating of the silicon tetrachloride that in polysilicon production process, produces hydrogenation takes place, obtain comprising the mixed gas of trichlorosilane, dichloro-dihydro silicon, hydrogenchloride and unreacted silicon tetrachloride that reaction generates, hydrogen, silica flour;
Purifying step: thus remove the Purge gas that silica flour in the mixed gas obtains comprising chlorosilane with chlorosilane;
Condensing steps: Purge gas is introduced heat exchange cooling in the rectifying tower tower bottom reboiler, and the Purge gas after the cooling is introduced condensing surface and is carried out condensation, obtains condensed fluid and noncondensable gas; Noncondensable gas is returned hydrogenation reactor, condensed fluid is sent into rectifying tower;
Rectification step: will be at the raw material of the isolated gas of rectifying tower cat head as polycrystalline silicon reducing furnace; To return hydrogenation reactor at the isolated liquid of rectifying Tata still.
Said condensed fluid can comprise trichlorosilane, silicon tetrachloride, dichloro-dihydro silicon and chlorosilane, and noncondensable gas can comprise hydrogen and hydrogenchloride.In rectification step, be silicon tetrachloride from the isolated liquid of rectifying Tata still, be trichlorosilane and dichloro-dihydro silicon from the isolated gas of rectifying tower cat head.
Preferably; In the above-mentioned method; Rectification step can also comprise: the liquid chlorosilane is vaporized through the rectifying tower tower bottom reboiler, and upwards transportation is as the thermal source of trichlorosilane and the vaporization of dichloro-dihydro silicon along rectifying tower, and vapor phase is discharged from tower bottom reboiler after becoming condensed fluid.The liquid chlorosilane of preferably, from tower bottom reboiler, discharging is delivered to condensing surface as heat-eliminating medium.
In the above-mentioned method, rectification step can also comprise: through the rectifying tower overhead condenser trichlorosilane is separated with dichloro-dihydro silicon, and with feedstock purification or the storage of trichlorosilane as polycrystalline silicon reducing furnace.
According to another aspect of the present invention, the device of Btu utilization in a kind of polysilicon production process is provided, has comprised
Hydrogenation reactor is used for introducing with silica flour, hydrogen with at the silicon tetrachloride that polysilicon production process produces that reaction generates trichlorosilane, dichloro-dihydro silicon and hydrogenchloride in the said hydrogenation reactor;
The washing tower that is communicated with hydrogenation reactor will be removed from the silica flour the mixed gas that comprises trichlorosilane, dichloro-dihydro silicon, hydrogenchloride, silicon tetrachloride, hydrogen and silica flour that hydrogenation reactor is discharged with chlorosilane, obtain comprising the Purge gas of chlorosilane;
Rectifying tower with tower bottom reboiler, tower bottom reboiler is communicated with washing tower, is used for Purge gas through lowering the temperature with the tower bottom reboiler heat exchange; And
The condensing surface that is communicated with tower bottom reboiler; Purge gas condensation after the cooling that said condensing surface will receive from tower bottom reboiler obtains condensed fluid and noncondensable gas; Said condensing surface also is communicated with hydrogenation reactor and rectifying tower respectively; Be used for noncondensable gas is returned hydrogenation reactor, condensed fluid is sent into rectifying tower, said rectifying Tata still is communicated with hydrogenation reactor.
Said condensed fluid comprises trichlorosilane, silicon tetrachloride, dichloro-dihydro silicon and chlorosilane, and noncondensable gas comprises hydrogen and hydrogenchloride.
Preferably, in the above-mentioned device, isolate silicon tetrachloride and return hydrogenation reactor from said rectifying Tata still; From the rectifying tower tower bottom reboiler, isolate chlorosilane and deliver to condensing surface as heat-eliminating medium.
Said rectifying tower can also comprise the condensing surface that is arranged on cat head.
The present invention both rationally utilized heat through Purge gas is delivered to condenser condenses earlier with after the rectifying tower reboiler heat exchange cooling again, alleviated the refrigerant load of condensing surface again.Chlorosilane is discharged the back directly as the heat-eliminating medium of condensing surface from the rectifying tower reboiler, both reduced energy consumption, makes rational use of resources again.There is following advantage at least in the present invention: 1) cold hydrogenation rectifying tower does not have steam consumption; 2) can condenser system refrigerant load be reduced by 34.8%; 3) the recirculated water cooler heat interchanging area in the condenser system reduces, and saves the equipment one-time investment; 4) quantity of circulating water reduces 40.6%, and then reduces water circulating pump load and cooling tower load.This shows that the present invention can significantly reduce production costs.
In addition, chlorosilane is met water can emit a large amount of heat, and is hydrolyzed into silicon-dioxide; Generate hydrogen ion and cl ions; Equipment there is very strong corrodibility, Serious Accident such as also possibly blast under the serious situation, and in the present invention; Can accident not continued to enlarge even reboiler is revealed also, and can learn leakage in advance through the variation of rectifying tower pressure.
Description of drawings
Fig. 1 is a traditional cold hydrogenation process schema.
Fig. 2 is a cold hydrogenation process schema of the present invention.
Embodiment
For the purpose, technical scheme and the advantage that make the embodiment of the invention is clearer, will combine accompanying drawing that specific embodiment is described in detail below.
As shown in Figure 2, the device of Btu utilization comprises in the polysilicon production process of the present invention: hydrogenation reactor 1; The washing tower 2 that is communicated with hydrogenation reactor 1; Rectifying tower 3 with tower bottom reboiler and overhead condenser, tower bottom reboiler is communicated with washing tower 2; And the condensing surface 4 that is communicated with tower bottom reboiler, this condensing surface 4 also is communicated with hydrogenation reactor 1 and rectifying tower 3 respectively, and rectifying tower 3 tower stills are communicated with hydrogenation reactor 1.Rectifying tower 3 cats head or overhead condenser can be communicated with polycrystalline silicon reducing furnace raw material storage device (not shown), or are communicated with the equipment of further purification.
The method of Btu utilization in the polysilicon production process of the present invention is described below.
For making full use of the heat energy in the hydrogenation gas, the present invention provides a kind of new technological process that is different from traditional technology, referring to Fig. 2, makes that the heat energy in the hydrogenation gas is utilized effectively.
Hydrogen and silicon tetrachloride are heated to 590-610 ℃; Be introduced into hydrogenation reactor 1 after being preferably 600 ℃; After reacting with silica flour in the hydrogenation reactor 1, obtain comprising the mixed gas of trichlorosilane, dichloro-dihydro silicon, hydrogenchloride and unreacted silicon tetrachloride that reaction generates, hydrogen, silica flour.
Above-mentioned mixed gas is imported washing tower 2, thereby obtain comprising the Purge gas of chlorosilane with the silica flour in the chlorosilane removal mixed gas.Purge gas is introduced heat exchange cooling in the tower bottom reboiler of rectifying tower 3, the Purge gas after the cooling is introduced condensing surface 4.From condensing surface 4, separate and obtain condensed fluid and noncondensable gas; Wherein, condensed fluid comprises trichlorosilane, silicon tetrachloride, dichloro-dihydro silicon and chlorosilane, and noncondensable gas comprises hydrogen and hydrogenchloride.The noncondensable gas that comprises hydrogen returns hydrogenation reactor 1 and recycles.Condensed fluid is then sent into rectifying tower 3.Send into the lower procedure of production of polysilicon at isolated gas trichlorosilane of rectifying tower 3 cats head and dichloro-dihydro silicon, or it is subsequent use to send in the polycrystalline silicon reducing furnace raw material storage device storage.As preferably; Also can use rectifying tower 3 overhead condensers that trichlorosilane is separated with dichloro-dihydro silicon, then that isolated purity is higher trichlorosilane is sent into polycrystalline silicon reducing furnace raw material storage device or is directly sent into polycrystalline silicon reducing furnace as the raw material of polycrystalline silicon reducing furnace.Returning hydrogenation reactor 1 in the isolated silicon tetrachloride liquid of rectifying tower 3 tower stills recycles.And the liquid chlorosilane passes through the vaporization of rectifying tower 3 tower bottom reboilers, and upwards transportation is as the thermal source of trichlorosilane and the vaporization of dichloro-dihydro silicon along rectifying tower 3, and vapor phase is delivered to condensing surface 4 as heat-eliminating medium from the tower bottom reboiler discharge after becoming condensed fluid.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (10)
1. the method for Btu utilization in the polysilicon production process comprises:
Synthesis step: with being incorporated in the hydrogenation reactor that is loaded with silica flour after hydrogen and the heating of the silicon tetrachloride that in polysilicon production process, produces hydrogenation takes place, obtain comprising the mixed gas of trichlorosilane, dichloro-dihydro silicon, hydrogenchloride and unreacted silicon tetrachloride that reaction generates, hydrogen, silica flour;
Purifying step: thus remove the Purge gas that silica flour in the mixed gas obtains comprising chlorosilane with chlorosilane;
Condensing steps: Purge gas is introduced heat exchange cooling in the rectifying tower tower bottom reboiler, and the Purge gas after the cooling is introduced condensing surface and is carried out condensation, obtains condensed fluid and noncondensable gas; Noncondensable gas is returned hydrogenation reactor, condensed fluid is sent into rectifying tower;
Rectification step: will be at the raw material of the isolated gas of rectifying tower cat head as polycrystalline silicon reducing furnace; To return hydrogenation reactor at the isolated liquid of rectifying Tata still.
2. method according to claim 1 is characterized in that, said condensed fluid comprises trichlorosilane, silicon tetrachloride, dichloro-dihydro silicon and chlorosilane, and noncondensable gas comprises hydrogen and hydrogenchloride.
3. method according to claim 2 is characterized in that, in rectification step, is silicon tetrachloride from the isolated liquid of rectifying Tata still, is trichlorosilane and dichloro-dihydro silicon from the isolated gas of rectifying tower cat head.
4. method according to claim 3; It is characterized in that; Rectification step also comprises: the liquid chlorosilane is vaporized through the rectifying tower tower bottom reboiler, and upwards transportation is as the thermal source of trichlorosilane and the vaporization of dichloro-dihydro silicon along rectifying tower, and vapor phase is discharged from tower bottom reboiler after becoming condensed fluid.
5. method according to claim 4 is characterized in that, the liquid chlorosilane of from tower bottom reboiler, discharging is delivered to condensing surface as heat-eliminating medium.
6. method according to claim 3 is characterized in that rectification step also comprises: through the rectifying tower overhead condenser trichlorosilane separated with dichloro-dihydro silicon, and with feedstock purification or the storage of trichlorosilane as polycrystalline silicon reducing furnace.
7. the device of Btu utilization in the polysilicon production process comprises
Hydrogenation reactor is used for introducing with silica flour, hydrogen with at the silicon tetrachloride that polysilicon production process produces that reaction generates trichlorosilane, dichloro-dihydro silicon and hydrogenchloride in the said hydrogenation reactor;
The washing tower that is communicated with hydrogenation reactor will be removed from the silica flour the mixed gas that comprises trichlorosilane, dichloro-dihydro silicon, hydrogenchloride, silicon tetrachloride, hydrogen and silica flour that hydrogenation reactor is discharged with chlorosilane, obtain comprising the Purge gas of chlorosilane;
Rectifying tower with tower bottom reboiler, tower bottom reboiler is communicated with washing tower, is used for Purge gas through lowering the temperature with the tower bottom reboiler heat exchange; And
The condensing surface that is communicated with tower bottom reboiler; Purge gas condensation after the cooling that said condensing surface will receive from tower bottom reboiler obtains condensed fluid and noncondensable gas; Said condensing surface also is communicated with hydrogenation reactor and rectifying tower respectively; Be used for noncondensable gas is returned hydrogenation reactor, condensed fluid is sent into rectifying tower, said rectifying Tata still is communicated with hydrogenation reactor.
8. device according to claim 7 is characterized in that, said condensed fluid comprises trichlorosilane, silicon tetrachloride, dichloro-dihydro silicon and chlorosilane, and noncondensable gas comprises hydrogen and hydrogenchloride.
9. device according to claim 8 is characterized in that, isolates silicon tetrachloride and returns hydrogenation reactor from said rectifying Tata still; From the rectifying tower tower bottom reboiler, isolate chlorosilane and deliver to condensing surface as heat-eliminating medium.
10. device according to claim 8 is characterized in that said rectifying tower also comprises the condensing surface that is arranged on cat head.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103205786A CN102786055A (en) | 2012-09-03 | 2012-09-03 | Method and device for heat utilization in polycrystalline silicon production process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103205786A CN102786055A (en) | 2012-09-03 | 2012-09-03 | Method and device for heat utilization in polycrystalline silicon production process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896280A (en) * | 2014-03-27 | 2014-07-02 | 洛阳利尔中晶光伏材料有限公司 | Operation method of polycrystalline silicon cold hydrogenation |
| CN103950934A (en) * | 2014-03-31 | 2014-07-30 | 中国恩菲工程技术有限公司 | Polysilicon preparation apparatus |
| CN103950933A (en) * | 2014-03-31 | 2014-07-30 | 中国恩菲工程技术有限公司 | Polysilicon preparation method |
| CN107673360A (en) * | 2017-11-13 | 2018-02-09 | 浙江工业大学上虞研究院有限公司 | For preparing the chemical industry equipment of trichlorosilane |
| CN107720758A (en) * | 2017-11-13 | 2018-02-23 | 浙江工业大学上虞研究院有限公司 | Chemical industry production system |
| CN115744915A (en) * | 2022-12-01 | 2023-03-07 | 华陆工程科技有限责任公司 | Chlorosilane liquid treatment method and treatment device |
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| JP2006001804A (en) * | 2004-06-18 | 2006-01-05 | Sumitomo Titanium Corp | Method of manufacturing silicon chloride and method of manufacturing polycrystalline silicon using the same |
| CN101618874A (en) * | 2009-08-13 | 2010-01-06 | 洛阳世纪新源硅业科技有限公司 | Method for producing trichlorosilane by coldly hydrogenating silicon tetrachloride |
| CN102070145A (en) * | 2010-12-06 | 2011-05-25 | 特变电工新疆硅业有限公司 | Method and device for recycling heat energy in reduction exhaust in polysilicon production process |
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2012
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006001804A (en) * | 2004-06-18 | 2006-01-05 | Sumitomo Titanium Corp | Method of manufacturing silicon chloride and method of manufacturing polycrystalline silicon using the same |
| CN101618874A (en) * | 2009-08-13 | 2010-01-06 | 洛阳世纪新源硅业科技有限公司 | Method for producing trichlorosilane by coldly hydrogenating silicon tetrachloride |
| CN102070145A (en) * | 2010-12-06 | 2011-05-25 | 特变电工新疆硅业有限公司 | Method and device for recycling heat energy in reduction exhaust in polysilicon production process |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896280A (en) * | 2014-03-27 | 2014-07-02 | 洛阳利尔中晶光伏材料有限公司 | Operation method of polycrystalline silicon cold hydrogenation |
| CN103896280B (en) * | 2014-03-27 | 2016-02-17 | 洛阳利尔中晶光伏材料有限公司 | A kind of operation method of polysilicon cold hydrogenation |
| CN103950934A (en) * | 2014-03-31 | 2014-07-30 | 中国恩菲工程技术有限公司 | Polysilicon preparation apparatus |
| CN103950933A (en) * | 2014-03-31 | 2014-07-30 | 中国恩菲工程技术有限公司 | Polysilicon preparation method |
| CN107673360A (en) * | 2017-11-13 | 2018-02-09 | 浙江工业大学上虞研究院有限公司 | For preparing the chemical industry equipment of trichlorosilane |
| CN107720758A (en) * | 2017-11-13 | 2018-02-23 | 浙江工业大学上虞研究院有限公司 | Chemical industry production system |
| CN115744915A (en) * | 2022-12-01 | 2023-03-07 | 华陆工程科技有限责任公司 | Chlorosilane liquid treatment method and treatment device |
| CN115744915B (en) * | 2022-12-01 | 2024-01-23 | 华陆工程科技有限责任公司 | Treatment method and treatment device for chlorosilane liquid |
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Application publication date: 20121121 |