CN103435044A - Method for purifying and separating chlorosilane from polysilicon tail gas - Google Patents
Method for purifying and separating chlorosilane from polysilicon tail gas Download PDFInfo
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- CN103435044A CN103435044A CN2013103049195A CN201310304919A CN103435044A CN 103435044 A CN103435044 A CN 103435044A CN 2013103049195 A CN2013103049195 A CN 2013103049195A CN 201310304919 A CN201310304919 A CN 201310304919A CN 103435044 A CN103435044 A CN 103435044A
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Abstract
The invention relates to a tail gas purifying technology in polysilicon production. A single rectifying method is traditionally adopted to separate impurities from trichlorosilane and needs a large apparatus and a high running cost. The invention provides a purifying method combining a polysilicon reduction reaction with a rectification, hydrolysis rectification and adsorption technology. The purifying method provided by the invention comprises the following steps: cooling tail gas, rectifying condensed trichlorosilane in a rectifying tower, allowing obtained trichlorosilane to enter a hydrolysis rectifying tower, allowing condensed partial trichlorosilane to enter an adsorption column, allowing purified trichlorosilane to enter a trichlorosilane separation tower, collecting a trichlorosilane product at the top of the trichlorosilane separation tower, allowing discharged silicon tetrachloride to enter the rectifying tower for purification, and collecting a silicon tetrachloride product at the bottom of the rectifying tower. The method provided by the invention has the advantages of apparatus simplification, low running cost, and reduction of the polysilicon production cost by 10%.
Description
Technical field
The invention belongs to polysilicon tail gas purifies and separates technical field, the chlorosilane that is specifically related to produce carries out the technical field of purifies and separates.
Background technology
Polysilicon is the main raw material of manufacturing silicon polished, solar cell and HIGH-PURITY SILICON goods, is main, the most basic functional material of semi-conductor industry, electronics and information industry, solar-energy photo-voltaic cell industry.Polysilicon can be divided into metallurgical grade, solar level, electronic-grade by the purity classification.The production method of high purity polycrystalline silicon has: improved Siemens, silane thermal decomposition process, fluidized bed process, metallurgy method.Along with large-scale developing and utilizing of green energy resource sun power, the purposes of photovoltaic cell raw material polysilicon is more and more extensive.Producing the widest that the method for polysilicon uses with Siemens Method, in the process of producing polysilicon raw material trichlorosilane, can produce a large amount of silicon tetrachloride as by-product, how effectively to utilize these by products, is the key issue that the polysilicon industry can diverse development.
Along with globalization speed is accelerated day by day, the development that mechanics of communication, network technology are advanced by leaps and bounds, optical fiber is as the most important medium of beared information, its demand also along with people to the raising of network requirement and rapid growth.High purity silicon tetrachloride is the main raw material of making optical fiber, its purity directly affects the loss characteristic of optical fiber, cause the detrimental impurity of optical fiber absorption loss to mainly contain iron, brill, nickel, copper, manganese, chromium, vanadium, platinum and hydroxide radical, data at home and abroad is thought, in optical fiber, the total concn of harmful transition metal ion and hydroxide ion will be lower than 1,000,000/, and individual other ionic concn will be lower than 1/100000000th.Main process for purification has rectification method, absorption method, hydrolysis method, extraction process and complexometry etc.But fiber optic materials is different to requirement and the semiconductor material of detrimental impurity, and stricter than semiconductor material to a certain extent to the requirement of foreign matter content.The various components that may exist in general synthetic silicon tetrachloride coarse fodder are about more than 70 and plant.The simple rectification method that adopts is difficult to trace impurity is reached to optical fiber level level; Single absorption method treatment capacity is less, is difficult for forming suitability for industrialized production; Hydrolysis method, extraction process and complexometry need add external substance to carry out removal of impurities, are difficult to remove fully the impurity of introducing in application process.
Simultaneously, in polysilicon production process, contain a large amount of trichlorosilanes in tail gas, as the main raw material of producing high purity polycrystalline silicon, foreign matter content wherein affects the quality of polysilicon, and the removal of impurities of need being purified is re-used as raw material and is used for producing polysilicon.The impurity that tradition is separated in trichlorosilane adopts rectificating method to purify, but needs huge equipment to realize.
summary of the invention
The object of the invention is to provide a kind of polysilicon reduction reaction and rectifying, hydrolysis method, adsorption technology to organically combine, and by the chlorosilane in polysilicon tail gas, comprises the processing method of the chlorosilane purifying of trichlorosilane and silicon tetrachloride.
The present invention realizes that the technical scheme that above-mentioned purpose adopts is as follows:
1, reduction reaction tail gas, hydrogenation tail gas, building-up reactions tail gas in production of polysilicon, contain hydrogen, trichlorosilane, silicon tetrachloride, dichloro-dihydro silicon, hydrogenchloride, tail gas is undertaken cooling by coolant media, the chlorosilane in tail gas under condensation enters subsequent processing.
2, the chlorosilane under condensation enters rectifying tower, and tower reactor is used steam to heat vaporization, and tower top arranges water cooler, tower top row light constituent, and tower reactor re-scheduling component, side line extraction chlorosilane, enter subsequent processing.
Further, chlorosilane foreign matter content difference to some extent in reduction tail gas, hydrogenation tail gas and synthesis tail gas can increase rectifying tower according to foreign matter content before or after this side line rectifying tower, was removed the impurity in trichlorosilane and silicon tetrachloride;
3, from the chlorosilane of side line rectifying tower extraction, enter the hydrolysis rectifying tower, at feed entrance point, high-purity wet nitrogen is set, high-purity wet nitrogen and silicon tetrachloride are mixed in the hydrolysis rectifying tower, tower reactor arranges reboiler, steam is heating source, tower reactor re-scheduling component, tower top is by gas phase non-condensable gas row light constituent, and an overhead condensation chlorosilane part is as the backflow of tower, another part extraction chlorosilane, the top gaseous phase non-condensable gas is disposed to exhaust system by the trim the top of column surge tank;
Further, the hydrolysis rectifying tower arranges packing tower, and filler is non-metallic material, is lined with tetrafluoroethylene in inner wall of tower;
Another step optimization, high-purity wet nitrogen water-content is controlled at 800 ~ 10000ppm, and mole proportioning 1:20 ~ 1:100 of wet nitrogen and chlorosilane is mixed into rectifying tower;
4, the chlorosilane liquid produced that certainly is hydrolyzed the extraction of rectifying tower tower top enters the chlorosilane adsorption column, the impurity in the absorption chlorosilane, and the chlorosilane output of products after the chlorosilane adsorption column is purified enters subsequent processing;
5, the chlorosilane from chlorosilane adsorption column outlet output enters the chlorosilane knockout tower, discharges silicon tetrachloride at the bottom of tower, and the overhead extraction trichlorosilane products, do the raw material production polysilicon; At the bottom of tower, silicon tetrachloride enters subsequent processing again;
6, the silicon tetrachloride of exporting from the chlorosilane knockout tower enters rectifying tower and is purified, and separates and wherein contains micro-trichlorosilane light constituent, tower reactor extraction silicon tetrachloride product.
The technology that the present invention utilizes hydrolysis rectifying and absorbing process to combine, can reduce the purifying chlorosilane reaches the high purity polycrystalline silicon raw materials for production and adopts single distillation technology, expend huge equipment and working cost, the production of polysilicon cost at least reduces by 10%, and the silicon tetrachloride after purifying reaches optical fiber materials standard.
The accompanying drawing explanation
The technical process of chlorosilane in Fig. 1 purifies and separates polysilicon tail gas;
In figure: 1-polysilicon tail gas refrigerating unit; The 2-knockout drum; 3-chlorosilane transferpump; 4-rectifying tower A; 5-is hydrolyzed rectifying tower; 6-chlorosilane adsorption column; 7-chlorosilane knockout tower; 8-rectifying tower C.
embodiment
In a kind of purifies and separates polysilicon tail gas, the method for chlorosilane, comprise the steps:
Reduction reaction tail gas, hydrogenation tail gas, building-up reactions tail gas in step 1, production of polysilicon, contain hydrogen, trichlorosilane, silicon tetrachloride, dichloro-dihydro silicon, hydrogenchloride, tail gas enters 1 import of polysilicon tail gas refrigerating unit, through recirculated water, carry out coolingly, gas-liquid mixture enters knockout drum 2.
The tail gas of step 2, chlorine-containing silane enters knockout drum 2, and liquid chlorosilane is separated with uncooled tail gas, and uncooled tail gas is from knockout drum 2 top outlet outputs;
Step 3, the chlorosilane of exporting from knockout drum 2 lower part outlets are pressed into rectifying tower A4 through chlorosilane transferpump 3, tower reactor is used the steam mode to be heated, gas phase is carried out cooling through overhead condenser, enter return tank after cooling, a part is as the backflow of rectifying tower, and a part of row's light constituent to storage tank is collected; Tower reactor row is containing the silicon tetrachloride heavy constituent; Side line extraction chlorosilane, non-condensable gas is discharged through return tank;
Step 4, from the chlorosilane of rectifying tower A4 side line extraction, enter hydrolysis rectifying tower 5, pass into high-purity wet nitrogen on feeding line, water-content is controlled at 800 ~ 10000ppm, mole proportioning 1:20 ~ 1:100 of wet nitrogen and chlorosilane, high-purity wet nitrogen and chlorosilane are mixed in hydrolysis rectifying tower 5, it is heating source that tower reactor arranges steam, tower reactor re-scheduling component, top gaseous phase carries out cooling through overhead condenser, enter return tank after cooling, and a part is as the backflow of rectifying tower, part extraction chlorosilane, the tower top non-condensable gas gives off by return tank;
Step 5, the chlorosilane liquid produced that certainly is hydrolyzed rectifying tower 5 overhead extractions enter chlorosilane adsorption column 6, metallic impurity and nonmetallic impurity in the absorption chlorosilane, and the chlorosilane output of products after the chlorosilane adsorption column is purified enters subsequent processing;
Step 6, the chlorosilane of exporting from 6 outlets of chlorosilane adsorption column enter chlorosilane knockout tower 7, at the bottom of tower, separate and discharge silicon tetrachloride, and trim the top of column extraction trichlorosilane products, do the raw material production polysilicon; At the bottom of tower, silicon tetrachloride enters subsequent processing again;
Step 7, the silicon tetrachloride of exporting from chlorosilane knockout tower 7 enter rectifying tower C8 and are purified, the logical steam heating vaporization of tower reactor reboiler, and tower top is discharged the light constituent containing trichlorosilane, tower reactor extraction silicon tetrachloride product.Can be used as the raw material of optical fiber production.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment, the present invention is had been described in detail, for a person skilled in the art, its technical scheme that still can put down in writing aforementioned each embodiment is modified, or part technical characterictic wherein is equal to replacement.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (4)
1. the method for chlorosilane in a purifies and separates polysilicon tail gas, chlorosilane comprises trichlorosilane and silicon tetrachloride, it is characterized by the purifying process scheme as follows:
By hydrogen, trichlorosilane, silicon tetrachloride, dichloro-dihydro silicon, the hydrogenchloride in the reduction reaction tail gas produced in production of polysilicon, hydrogenation tail gas, building-up reactions tail gas, described above tail gas is undertaken cooling by coolant media, the chlorosilane in tail gas under condensation enters subsequent processing;
Chlorosilane under condensation enters rectifying tower, and tower reactor is used steam to carry out heating and gasifying, and tower top arranges water cooler, tower top row light constituent, and tower reactor re-scheduling component, side line extraction chlorosilane, enter subsequent processing;
The chlorosilane of side line rectifying tower extraction, enter the hydrolysis rectifying tower, at feed entrance point, high-purity wet nitrogen is set, high-purity wet nitrogen and silicon tetrachloride are mixed in the hydrolysis rectifying tower, tower reactor arranges reboiler, steam is heating source, tower reactor is discharged heavy constituent, and tower top is by gas phase non-condensable gas row light constituent, and an overhead condensation chlorosilane part is as the backflow of tower, another part extraction chlorosilane, the top gaseous phase non-condensable gas is disposed to exhaust system by the trim the top of column surge tank;
Chlorosilane liquid produced from the extraction of hydrolysis rectifying tower tower top enters the chlorosilane adsorption column, the impurity in the absorption chlorosilane, and the chlorosilane output of products after the chlorosilane adsorption column is purified enters subsequent processing;
Chlorosilane from chlorosilane adsorption column outlet output enters the chlorosilane knockout tower, discharges silicon tetrachloride at the bottom of tower, and the overhead extraction trichlorosilane products, do the raw material production polysilicon; At the bottom of tower, silicon tetrachloride enters subsequent processing again;
The silicon tetrachloride of exporting from the chlorosilane knockout tower enters rectifying tower and is purified, and separates the wherein trichlorosilane light constituent of trace, tower reactor extraction silicon tetrachloride product.
2. the method for chlorosilane in purifies and separates polysilicon tail gas according to claim 1, it is characterized by according to reduction tail gas, chlorosilane foreign matter content difference in hydrogenation tail gas and synthesis tail gas, in operation 2) rectifying tower front or back can increase rectifying tower, further remove the impurity in trichlorosilane and silicon tetrachloride.
3. the method for chlorosilane in purifies and separates polysilicon tail gas according to claim 1, is characterized by the hydrolysis rectifying tower packing tower be set, and filler is non-metallic material, is lined with tetrafluoroethylene in inner wall of tower.
4. the method for chlorosilane in purifies and separates polysilicon tail gas according to claim 1, the water content that it is characterized by the high-purity wet nitrogen that enters the hydrolysis rectifying tower is controlled at 800-10000ppm, and wet nitrogen is to enter the hydrolysis rectifying tower after 1:20-1:100 is mixed with mole proportioning of chlorosilane.
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Cited By (11)
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| CN105314638A (en) * | 2015-11-26 | 2016-02-10 | 新疆大全新能源有限公司 | Method and device for recycling silicon tetrachloride and removing high-boiling residues in trichlorosilane synthetic material |
| CN106573182A (en) * | 2014-10-09 | 2017-04-19 | 瓦克化学股份公司 | Purification of chlorosilanes by means of distillation and adsorption |
| CN107720759A (en) * | 2017-11-13 | 2018-02-23 | 亚洲硅业（青海）有限公司 | The processing method of tail gas is reduced in a kind of preparation method and production of polysilicon of optical fiber level silicon tetrachloride |
| CN109292780A (en) * | 2017-07-25 | 2019-02-01 | 江苏中能硅业科技发展有限公司 | A kind of technique of impurity removal reaction purification chlorosilane |
| CN109678158A (en) * | 2017-10-19 | 2019-04-26 | 新特能源股份有限公司 | Exhaust gas treating method and system in polysilicon production process |
| CN110627071A (en) * | 2019-11-12 | 2019-12-31 | 四川永祥新能源有限公司 | Polychlorosilane processing apparatus in polycrystalline silicon production |
| CN112642259A (en) * | 2020-12-23 | 2021-04-13 | 浙江天采云集科技股份有限公司 | Method for recovering FTrPSA (fluorine substituted PSA) tail gas generated in epitaxial process of chlorine-based SiC-CVD (chemical vapor deposition) by alkane and silane reaction |
| CN113401907A (en) * | 2020-03-16 | 2021-09-17 | 新疆新特晶体硅高科技有限公司 | Method and device for purifying and separating silicon tetrachloride in polycrystalline silicon synthesis |
| CN115092933A (en) * | 2022-05-16 | 2022-09-23 | 内蒙古鄂尔多斯电力冶金集团股份有限公司 | Processing system of electronic grade polycrystalline silicon reduction tail gas |
| CN116407861A (en) * | 2023-03-16 | 2023-07-11 | 清电光伏科技有限公司 | Fixed bed-based electronic grade polysilicon rectification carbon removal device and method |
| CN116495741A (en) * | 2023-05-31 | 2023-07-28 | 内蒙古润阳悦达新能源科技有限公司 | Method and system for recycling polysilicon production associated disilicide raw materials |
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| CN106573182B (en) * | 2014-10-09 | 2019-03-08 | 瓦克化学股份公司 | Chlorosilane purification is carried out by distilling and adsorbing |
| CN105314638B (en) * | 2015-11-26 | 2018-01-05 | 新疆大全新能源有限公司 | Silicon tetrachloride recycling and the method and apparatus except high-boiling components in trichlorosilane synthesis material |
| CN105314638A (en) * | 2015-11-26 | 2016-02-10 | 新疆大全新能源有限公司 | Method and device for recycling silicon tetrachloride and removing high-boiling residues in trichlorosilane synthetic material |
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| CN109292780A (en) * | 2017-07-25 | 2019-02-01 | 江苏中能硅业科技发展有限公司 | A kind of technique of impurity removal reaction purification chlorosilane |
| CN109678158A (en) * | 2017-10-19 | 2019-04-26 | 新特能源股份有限公司 | Exhaust gas treating method and system in polysilicon production process |
| CN107720759A (en) * | 2017-11-13 | 2018-02-23 | 亚洲硅业（青海）有限公司 | The processing method of tail gas is reduced in a kind of preparation method and production of polysilicon of optical fiber level silicon tetrachloride |
| CN110627071A (en) * | 2019-11-12 | 2019-12-31 | 四川永祥新能源有限公司 | Polychlorosilane processing apparatus in polycrystalline silicon production |
| CN110627071B (en) * | 2019-11-12 | 2021-08-10 | 四川永祥新能源有限公司 | Polychlorosilane processing apparatus in polycrystalline silicon production |
| CN113401907A (en) * | 2020-03-16 | 2021-09-17 | 新疆新特晶体硅高科技有限公司 | Method and device for purifying and separating silicon tetrachloride in polycrystalline silicon synthesis |
| CN112642259A (en) * | 2020-12-23 | 2021-04-13 | 浙江天采云集科技股份有限公司 | Method for recovering FTrPSA (fluorine substituted PSA) tail gas generated in epitaxial process of chlorine-based SiC-CVD (chemical vapor deposition) by alkane and silane reaction |
| CN115092933A (en) * | 2022-05-16 | 2022-09-23 | 内蒙古鄂尔多斯电力冶金集团股份有限公司 | Processing system of electronic grade polycrystalline silicon reduction tail gas |
| CN115092933B (en) * | 2022-05-16 | 2024-01-12 | 内蒙古鄂尔多斯电力冶金集团股份有限公司 | Treatment system for electronic grade polysilicon reduction tail gas |
| CN116407861A (en) * | 2023-03-16 | 2023-07-11 | 清电光伏科技有限公司 | Fixed bed-based electronic grade polysilicon rectification carbon removal device and method |
| CN116495741A (en) * | 2023-05-31 | 2023-07-28 | 内蒙古润阳悦达新能源科技有限公司 | Method and system for recycling polysilicon production associated disilicide raw materials |
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