CN103936009B - A kind of thermal decomposition of silane produces the device and method of nano level high-purity silicon powder - Google Patents
A kind of thermal decomposition of silane produces the device and method of nano level high-purity silicon powder Download PDFInfo
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- CN103936009B CN103936009B CN201410159327.3A CN201410159327A CN103936009B CN 103936009 B CN103936009 B CN 103936009B CN 201410159327 A CN201410159327 A CN 201410159327A CN 103936009 B CN103936009 B CN 103936009B
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Abstract
The invention discloses the device and method that a kind of thermal decomposition of silane produces nano level high-purity silicon powder.Comprise thermal decomposition of silane system, silica flour collecting by filtration system and tail gas recycle treatment system, described silane decomposes system comprises reaction gas silane pipeline, reaction gas hydrogen gas lines, proportioning surge tank, silane tubular reactor, exhaust gas cooler, silica flour collecting by filtration system comprises hydrogen power back-blowing filter pipeline, one-level silica flour strainer, secondary silica flour strainer, one-level silica flour collecting bin, secondary silica flour collecting bin, vacuum pump, one-level silica flour outlet line, secondary silica flour outlet line, tail gas recycle treatment system comprises tail gas cryogenic device, compressor, adsorption tower, knockout drum, the liquid silane outlet line of knockout drum, knockout drum hydrogen outlet pipeline.The present invention is applicable to the production of industrial nano grade high-purity silicon powder, and can collection cut size be effectively the silica flour of more than 30nm, tail gas all reclaims use, non-pollution discharge, has the advantages such as less investment, cost be low.
Description
Technical field
The present invention relates to the device and method that a kind of thermal decomposition of silane produces nano level high-purity silicon powder.
Background technology
Nano silica fume is a kind of brownish-yellow powder, of many uses.Can be used as charged lithium cells negative material, improve lithium battery capacity and charge and discharge cycles number of times, also can be used in fire-resistant coating and refractory materials, have huge potential application foreground in fields such as stupalith, matrix material, catalytic material, photoelectric material and biomaterials simultaneously.
Nano silica fume production technique conventional at present has electrostatic spray assisted chemical deposition (ES-CVD), hot-wire chemical gas-phase deposition (HWCVD), laser-induced chemical vapour deposition (LICVD) etc., but these methods are high to equipment requirements, energy consumption is large, and is difficult to realize industrialization production.
Summary of the invention
The object of the invention is to overcome that existing nano level high-purity silicon powder production technique cost is high, energy consumption large and the deficiency such as industrialization, the device and method that a kind of equipment is simple, the thermal decomposition of silane of operational safety produces nano level high-purity silicon powder is provided, closed cycle continuous seepage can be realized, cost is low, and production capacity is high.
The device that a kind of thermal decomposition of silane produces nano level high-purity silicon powder comprises thermal decomposition of silane system, silica flour collecting by filtration system and tail gas recycle treatment system, described silane decomposes system comprises reaction gas silane pipeline, reaction gas hydrogen gas lines, proportioning surge tank, silane tubular reactor, exhaust gas cooler, reaction gas silane pipeline, reaction gas hydrogen gas lines is connected with proportioning surge tank, proportioning surge tank, silane tubular reactor, exhaust gas cooler is connected in turn, and silica flour collecting by filtration system comprises hydrogen power back-blowing filter pipeline, one-level silica flour strainer, secondary silica flour strainer, one-level silica flour collecting bin, secondary silica flour collecting bin, vacuum pump, one-level silica flour outlet line, secondary silica flour outlet line, hydrogen power back-blowing filter pipeline one end is connected with reaction gas hydrogen gas lines, the hydrogen power back-blowing filter pipeline the other end respectively with one-level silica flour strainer, secondary silica flour strainer is connected, exhaust gas cooler, one-level silica flour strainer, secondary silica flour strainer is connected in turn, one-level silica flour strainer, one-level silica flour collecting bin, one-level silica flour outlet line is connected in turn, secondary silica flour strainer, secondary silica flour collecting bin, secondary silica flour outlet line is connected in turn, one-level silica flour collecting bin, secondary silica flour collecting bin is connected with vacuum pump respectively, and tail gas recycle treatment system comprises tail gas cryogenic device, compressor, adsorption tower, knockout drum, the liquid silane outlet line of knockout drum, knockout drum hydrogen outlet pipeline, secondary silica flour strainer, tail gas cryogenic device, compressor, adsorption tower, knockout drum, the liquid silane outlet line of knockout drum is connected in turn, and knockout drum is connected with proportioning surge tank by knockout drum hydrogen outlet pipeline.
The method that nano level high-purity silicon powder is produced in described device thermolysis comprises the steps:
1) high purity silane and high-purity hydrogen enter proportioning surge tank and carry out mixing match, obtain gas mixture;
2) gas mixture enters silane tubular reactor, and in silane tubular reactor, silane thermal degradation granulates silica flour and hydrogen, and the outlet of silane tubular reactor obtains gas powder gas mixture;
3) reacted gas powder gas mixture is after exhaust gas cooler cooling, and temperature is down to less than 100 DEG C, enters one-level silica flour strainer, is leached by silica flour, is collected in one-level silica flour filter bottom;
4) high-purity hydrogen that the silica flour being adsorbed on filter membrane outside uses hydrogen power back-blowing filter pipeline to provide carries out reverse blowing disposal;
5) after one-level silica flour strainer reaches the silica flour of specified quantity, close one-level silica flour strainer, open secondary silica flour strainer, allow exhaust gas cooler cooled gas powder gas mixture enter secondary silica flour strainer and continue to produce;
6) replace one-level silica flour strainer: collect feed bin with vacuum pump to one-level silica flour and vacuumize process, feed bin collected by connection one-level silica flour strainer and one-level silica flour, silica flour put into one-level silica flour and collect feed bin,
7) after secondary silica flour strainer reaches the silica flour of specified quantity, enable the one-level silica flour strainer after displacement, and replacement operator is carried out to secondary silica flour strainer, realize one-level silica flour strainer and secondary silica flour strainer switching use, make reaction have continuity; Described carries out replacement operator for vacuumize process with vacuum pump to secondary silica flour strainer to secondary silica flour strainer, and feed bin collected by connection secondary silica flour strainer and secondary silica flour, silica flour is put into secondary silica flour and collects feed bin;
8) tail gas after one-level silica flour strainer or secondary silica flour metre filter enters tail gas recycle treatment system, after the cooling of tail gas cryogenic device, compressor compresses, absorption tower adsorbs, at knockout drum by silane and Hydrogen Separation, separating obtained hydrogen fills into proportioning surge tank by knockout drum hydrogen outlet pipeline, and separating obtained silane is purified.
Described high purity silane and the purity of high-purity hydrogen are greater than 99.9999%.
In described gas mixture, the volumetric molar concentration of silane is 5% ~ 20%, and the pressure of gas mixture maintains 0.3Mpa, enters the flow control of reactor at 80-100kg/h after silane and hydrogen proportioning.
The thermal degradation temperature of described silane controls at 500 DEG C ~ 900 DEG C.The thermal degradation temperature of silane described further controls at 500 DEG C ~ 600 DEG C.
Described silane tubular reactor is provided with one section of constant temperature hot-zone, and Heating temperature can be made constant in 0 ~ 1200 DEG C.
Described exhaust gas cooler uses circulating cooling water cooling, and reacted gas powder mixture temperature can be made to be down to less than 100 DEG C.
Described hydrogen power back-blowing filter pipeline gos deep into one-level silica flour strainer and secondary silica flour filter center, the silica flour that reverse blow strainer adsorbs outward.
Described tail gas recycle treatment system adopts cryogenic liquid refrigerated separation silane and hydrogen, and described cryogenic liquid is liquid nitrogen.
The present invention is applicable to the production of industrial nano grade high-purity silicon powder, and tail gas is all recycled, non-pollution discharge, has less investment, low cost and other advantages.
Accompanying drawing explanation
Fig. 1 is the structural representation that thermal decomposition of silane produces nano level high-purity silicon powder device;
Fig. 2 is the SEM photo of temperature of reaction at 880 DEG C of silica flours produced;
Fig. 3 is the SEM photo of temperature of reaction at 500 DEG C of silica flours produced;
Fig. 4 is the SEM photo of temperature of reaction at 750 DEG C of silica flours produced;
Fig. 5 is the SEM photo of temperature of reaction at 600 DEG C of silica flours produced;
In figure, should gas silane pipeline 1, reaction gas hydrogen gas lines 2, proportioning surge tank 3, silane tubular reactor 4, exhaust gas cooler 5, hydrogen power back-blowing filter pipeline 6, one-level silica flour strainer 7, secondary silica flour strainer 8, one-level silica flour collecting bin 9, secondary silica flour collecting bin 10, vacuum pump 11, one-level silica flour outlet line 12, secondary silica flour outlet line 13, tail gas cryogenic device 14, compressor 15, adsorption tower 16, knockout drum 17, the liquid silane outlet line 18 of knockout drum, knockout drum hydrogen outlet pipeline 19.
Embodiment
As shown in Figure 1, a kind of device of thermal decomposition of silane production nano level high-purity silicon powder comprises thermal decomposition of silane system, silica flour collecting by filtration system and tail gas recycle treatment system, described silane decomposes system comprises reaction gas silane pipeline 1, reaction gas hydrogen gas lines 2, proportioning surge tank 3, silane tubular reactor 4, exhaust gas cooler 5, reaction gas silane pipeline 1, reaction gas hydrogen gas lines 2 is connected with proportioning surge tank 3, proportioning surge tank 3, silane tubular reactor 4, exhaust gas cooler 5 is connected in turn, and silica flour collecting by filtration system comprises hydrogen power back-blowing filter pipeline 6, one-level silica flour strainer 7, secondary silica flour strainer 8, one-level silica flour collecting bin 9, secondary silica flour collecting bin 10, vacuum pump 11, one-level silica flour outlet line 12, secondary silica flour outlet line 13, hydrogen power back-blowing filter pipeline 6 one end is connected with reaction gas hydrogen gas lines 2, hydrogen power back-blowing filter pipeline 6 the other end respectively with one-level silica flour strainer 7, secondary silica flour strainer 8 is connected, exhaust gas cooler 5, one-level silica flour strainer 7, secondary silica flour strainer 8 is connected in turn, one-level silica flour strainer 7, one-level silica flour collecting bin 9, one-level silica flour outlet line 12 is connected in turn, secondary silica flour strainer 8, secondary silica flour collecting bin 10, secondary silica flour outlet line 13 is connected in turn, one-level silica flour collecting bin 9, secondary silica flour collecting bin 10 is connected with vacuum pump 11 respectively, and tail gas recycle treatment system comprises tail gas cryogenic device 14, compressor 15, adsorption tower 16, knockout drum 17, the liquid silane outlet line 18 of knockout drum, knockout drum hydrogen outlet pipeline 19, secondary silica flour strainer 8, tail gas cryogenic device 14, compressor 15, adsorption tower 16, knockout drum 17, the liquid silane outlet line 18 of knockout drum is connected in turn, and knockout drum 17 is connected with proportioning surge tank 3 by knockout drum hydrogen outlet pipeline 19.
Described silane tubular reactor 4 has one section of constant temperature hot-zone, can make Heating temperature constant between 0 ~ 1200 DEG C arbitrary temperature.
Described exhaust gas cooler 5 uses circulating cooling water cooling, and reacted gas powder mixture temperature can be made to be down to less than 100 DEG C.
Described hydrogen power back-blowing filter pipeline 6 gos deep into one-level silica flour strainer 7 and secondary silica flour strainer 8 center, the silica flour that reverse blow strainer adsorbs outward.
Described tail gas recycle treatment system adopts cryogenic liquid refrigerated separation silane and hydrogen, and described cryogenic liquid is liquid nitrogen.
The silica flour stored in one-level silica flour collecting bin 9, secondary silica flour collecting bin 10 can respectively by one-level silica flour outlet line 12, the discharging of secondary silica flour outlet line 13.
embodiment 1:
Be that the high-purity hydrogen of high purity silane 500kg and the 6N of 6N carries out Homogeneous phase mixing according to the ratio that volumetric molar concentration is 20% purity, and enter into 880 DEG C according to mixed total amount 100kg/h, pressure is the silane tubular reactor thermal degradation of 0.30Mpa, generate microgranular silica flour and unreacted tail gas through overcooling laggard enter to silica flour strainer, after filtering, tail gas enters tail gas recycle treatment system, through overcooling, compression, after absorption, by silane and Hydrogen Separation, separating obtained hydrogen fills into proportioning surge tank, separating obtained silane comes back to silane scavenging tower and carries out purification in order to re-using.The silica flour produced is after one-level silica flour collecting bin and secondary silica flour collecting bin are collected, and obtain the silica flour 314kg of 150nm ~ 350nm, a transformation efficiency of silane is 71.78%, and the SEM photo obtained is as Fig. 2.
embodiment 2:
Be that the high-purity hydrogen of high purity silane 500kg and the 6N of 6N carries out Homogeneous phase mixing according to the ratio that volumetric molar concentration is 5% purity, and enter into 500 DEG C according to mixed total amount 80kg/h, pressure is the silane tubular reactor thermal degradation of 0.30Mpa, generate microgranular silica flour and unreacted tail gas through overcooling laggard enter to silica flour strainer, after filtering, tail gas enters tail gas recycle treatment system, through overcooling, compression, after absorption, by silane and Hydrogen Separation, separating obtained hydrogen fills into proportioning surge tank, separating obtained silane comes back to silane scavenging tower and carries out purification in order to re-using.The silica flour produced is after one-level silica flour collecting bin and secondary silica flour collecting bin are collected, and obtain the silica flour 178kg of 30nm ~ 90nm, a transformation efficiency of silane is 40.69%, and the SEM photo obtained is as Fig. 3.
embodiment 3:
Be that the high-purity hydrogen of high purity silane 500kg and the 6N of 6N carries out Homogeneous phase mixing according to the ratio that volumetric molar concentration is 15% purity, and enter into 750 DEG C according to mixed total amount 80kg/h, pressure is the silane tubular reactor thermal degradation of 0.30Mpa, generate microgranular silica flour and unreacted tail gas through overcooling laggard enter to silica flour strainer, after filtering, tail gas enters tail gas recycle treatment system, through overcooling, compression, after absorption, by silane and Hydrogen Separation, separating obtained hydrogen fills into proportioning surge tank, separating obtained silane comes back to silane scavenging tower and carries out purification in order to re-using.The silica flour produced is after one-level silica flour collecting bin and secondary silica flour collecting bin are collected, and obtain the silica flour 262kg of 50nm ~ 250nm, a transformation efficiency of silane is 59.89%, and the SEM photo obtained is as Fig. 4.
embodiment 4:
Be that the high-purity hydrogen of high purity silane 500kg and the 6N of 6N carries out Homogeneous phase mixing according to the ratio that volumetric molar concentration is 10% purity, and enter into 600 DEG C according to mixed total amount 90kg/h, pressure is the silane tubular reactor thermal degradation of 0.30Mpa, generate microgranular silica flour and unreacted tail gas through overcooling laggard enter to silica flour strainer, after filtering, tail gas enters tail gas recycle treatment system, through overcooling, compression, after absorption, by silane and Hydrogen Separation, separating obtained hydrogen fills into proportioning surge tank, separating obtained silane comes back to silane scavenging tower and carries out purification in order to re-using.The silica flour produced is after one-level silica flour collecting bin and secondary silica flour collecting bin are collected, and obtain the silica flour 231kg of 30nm ~ 120nm, a transformation efficiency of silane is 52.80%, and the SEM photo obtained is as Fig. 5.
Claims (9)
1. a method for nano level high-purity silicon powder is produced in device for carrying out said thermolysis, it is characterized in that comprising the steps:
1) high purity silane and high-purity hydrogen enter proportioning surge tank (3) and carry out mixing match, obtain gas mixture;
2) gas mixture enters silane tubular reactor (4), and in silane tubular reactor (4), silane thermal degradation granulates silica flour and hydrogen, and the outlet of silane tubular reactor (4) obtains gas powder gas mixture;
3) reacted gas powder gas mixture is after exhaust gas cooler (5) cooling, and temperature is down to less than 100 DEG C, enters one-level silica flour strainer (7), is leached by silica flour, is collected in one-level silica flour strainer (7) bottom;
4) high-purity hydrogen that the silica flour being adsorbed on filter membrane outside uses hydrogen power back-blowing filter pipeline (6) to provide carries out reverse blowing disposal;
5) after one-level silica flour strainer (7) reaches the silica flour of specified quantity, close one-level silica flour strainer (7), open secondary silica flour strainer (8), allow exhaust gas cooler (5) cooled gas powder gas mixture enter secondary silica flour strainer (8) and continue to produce;
6) one-level silica flour strainer (7) is replaced: with vacuum pump (11), feed bin (9) is collected to one-level silica flour and vacuumize process, be communicated with one-level silica flour strainer (7) and collect feed bin (9) with one-level silica flour, silica flour is put into one-level silica flour and collect feed bin (9);
7) after secondary silica flour strainer (8) reaches the silica flour of specified quantity, enable the one-level silica flour strainer (7) after displacement, and replacement operator is carried out to secondary silica flour strainer (8), realize one-level silica flour strainer (7) and secondary silica flour strainer (8) switching use, make reaction have continuity; Described carries out replacement operator for vacuumize process with vacuum pump (11) to secondary silica flour strainer (8) to secondary silica flour strainer (8), be communicated with secondary silica flour strainer (8) and collect feed bin (10) with secondary silica flour, silica flour is put into secondary silica flour and collect feed bin (10);
8) tail gas after one-level silica flour strainer (7) or secondary silica flour strainer (8) filter enters tail gas recycle treatment system, after tail gas cryogenic device (14) cooling, compressor (15) compression, adsorption tower (16) absorption, at knockout drum (17) by silane and Hydrogen Separation, separating obtained hydrogen fills into proportioning surge tank (3) by knockout drum hydrogen outlet pipeline (19), and separating obtained silane is purified;
Described device comprises thermal decomposition of silane system, silica flour collecting by filtration system and tail gas recycle treatment system, described silane decomposes system comprises reaction gas silane pipeline (1), reaction gas hydrogen gas lines (2), proportioning surge tank (3), silane tubular reactor (4), exhaust gas cooler (5), reaction gas silane pipeline (1), reaction gas hydrogen gas lines (2) is connected with proportioning surge tank (3), proportioning surge tank (3), silane tubular reactor (4), exhaust gas cooler (5) is connected in turn, and silica flour collecting by filtration system comprises hydrogen power back-blowing filter pipeline (6), one-level silica flour strainer (7), secondary silica flour strainer (8), one-level silica flour collecting bin (9), secondary silica flour collecting bin (10), vacuum pump (11), one-level silica flour outlet line (12), secondary silica flour outlet line (13), hydrogen power back-blowing filter pipeline (6) one end is connected with reaction gas hydrogen gas lines (2), hydrogen power back-blowing filter pipeline (6) the other end respectively with one-level silica flour strainer (7), secondary silica flour strainer (8) is connected, exhaust gas cooler (5), one-level silica flour strainer (7), secondary silica flour strainer (8) is connected in turn, one-level silica flour strainer (7), one-level silica flour collecting bin (9), one-level silica flour outlet line (12) is connected in turn, secondary silica flour strainer (8), secondary silica flour collecting bin (10), secondary silica flour outlet line (13) is connected in turn, one-level silica flour collecting bin (9), secondary silica flour collecting bin (10) is connected with vacuum pump (11) respectively, and tail gas recycle treatment system comprises tail gas cryogenic device (14), compressor (15), adsorption tower (16), knockout drum (17), liquid silane outlet line (18) of knockout drum, knockout drum hydrogen outlet pipeline (19), secondary silica flour strainer (8), tail gas cryogenic device (14), compressor (15), adsorption tower (16), knockout drum (17), liquid silane outlet line (18) of knockout drum is connected in turn, and knockout drum (17) is connected with proportioning surge tank (3) by knockout drum hydrogen outlet pipeline (19).
2. the thermal decomposition of silane according to right 1 produces the method for nano level high-purity silicon powder, it is characterized in that the purity of described high purity silane and high-purity hydrogen is greater than 99.9999%.
3. the thermal decomposition of silane according to right 1 produces the method for nano level high-purity silicon powder, it is characterized in that the volumetric molar concentration of silane in described gas mixture is 5% ~ 20%, the pressure of gas mixture maintains 0.3Mpa, enters the flow control of reactor at 80-100kg/h after silane and hydrogen proportioning.
4. the thermal decomposition of silane according to right 1 produces the method for nano level high-purity silicon powder, it is characterized in that the thermal degradation temperature of described silane controls at 500 DEG C ~ 900 DEG C.
5. the thermal decomposition of silane according to right 1 produces the method for nano level high-purity silicon powder, it is characterized in that the thermal degradation temperature of described silane controls at 500 DEG C ~ 600 DEG C.
6. the thermal decomposition of silane according to right 1 produces the method for nano level high-purity silicon powder, it is characterized in that described silane tubular reactor (4) is provided with one section of constant temperature hot-zone, Heating temperature can be made constant in 0 ~ 1200 DEG C.
7. the thermal decomposition of silane according to right 1 produces the method for nano level high-purity silicon powder, it is characterized in that described exhaust gas cooler (5) uses circulating cooling water cooling, reacted gas powder mixture temperature can be made to be down to less than 100 DEG C.
8. the thermal decomposition of silane according to right 1 produces the method for nano level high-purity silicon powder, it is characterized in that described hydrogen power back-blowing filter pipeline (6) gos deep into one-level silica flour strainer (7) and secondary silica flour strainer (8) center, the silica flour that reverse blow strainer adsorbs outward.
9. the thermal decomposition of silane according to right 1 produces the method for nano level high-purity silicon powder, and it is characterized in that described tail gas recycle treatment system adopts cryogenic liquid refrigerated separation silane and hydrogen, described cryogenic liquid is liquid nitrogen.
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| CN114031082B (en) * | 2021-12-22 | 2023-10-31 | 中国有色桂林矿产地质研究院有限公司 | Method for preparing nano silicon powder by induction plasma pyrolysis of silane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102046529A (en) * | 2008-03-31 | 2011-05-04 | 施米德硅晶片科技有限责任公司 | Method and system for the production of pure silicon |
| WO2013025707A1 (en) * | 2011-08-15 | 2013-02-21 | Dow Corning Corporation | Electrode composition comprising a silicon powder and method of controlling the crystallinity of a silicon powder |
| CN203794640U (en) * | 2014-04-21 | 2014-08-27 | 浙江中宁硅业有限公司 | Device for producing nanoscale high-purity silicon powder through silane thermal decomposition |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102046529A (en) * | 2008-03-31 | 2011-05-04 | 施米德硅晶片科技有限责任公司 | Method and system for the production of pure silicon |
| WO2013025707A1 (en) * | 2011-08-15 | 2013-02-21 | Dow Corning Corporation | Electrode composition comprising a silicon powder and method of controlling the crystallinity of a silicon powder |
| CN203794640U (en) * | 2014-04-21 | 2014-08-27 | 浙江中宁硅业有限公司 | Device for producing nanoscale high-purity silicon powder through silane thermal decomposition |
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