CN102818439A - Drying device and drying method for high-purity silicon materials - Google Patents
Drying device and drying method for high-purity silicon materials Download PDFInfo
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- CN102818439A CN102818439A CN2012103154892A CN201210315489A CN102818439A CN 102818439 A CN102818439 A CN 102818439A CN 2012103154892 A CN2012103154892 A CN 2012103154892A CN 201210315489 A CN201210315489 A CN 201210315489A CN 102818439 A CN102818439 A CN 102818439A
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Abstract
The invention discloses a drying device for high-purity silicon materials. The drying device comprises a case. The case is a sealed case with a sealing door, multiple layers of drying plate supports are arranged in an inner cavity of the case, toothed rails are arranged on each layer of drying plate supports, and drying plates are disposed on the toothed rails; two vacuum breaking ports are respectively arranged on side walls of the case; the case is communicated with a vacuumizing device via a vacuumizing port on a side wall, is communicated with a vacuum gauge via a vacuum verifying hole on the side wall and is communicated with a medium circulating heating device via a heat-conduction medium inlet and a heat-conduction medium outlet on the side wall simultaneously; and the vacuumizing device and the medium circulating heating device are respectively connected with a control device via signals. The invention further discloses a drying method for the high-purity silicon materials. The drying method includes placing the to-be-dried high-purity silicon materials in the sealed case; vacuumizing the case by a vacuum pump; heating to dry the high-purity silicon materials; detecting a drying effect in real time; and heating the high-purity silicon materials until technical requirements are met. The drying device and the drying method have the advantages of simple structure and high drying efficiency.
Description
Technical field
The present invention relates to solar power silicon material drying technology field, relate to a kind of HIGH-PURITY SILICON material drying unit, the invention still further relates to the method for utilizing this kind device that the HIGH-PURITY SILICON material is dried.
Background technology
At present, high purity polycrystalline silicon material commonly used mainly contains quick-fried block of material of water, bulk material, particle polycrystal material, fragment material, flaw-piece material etc., cleans the back and adopts constant temperature air blast mode to dry.In the drying course, because the polycrystalline silicon material kind is more, size is inhomogeneous, and the common drying baker oven dry time spent reaches 30-60min, and bake out temperature is at 180-200 ℃, and drying course is slow, and energy consumption is big, and drying efficiency is lower; And in drying course, can pollute the material surface, reduce feed purity, influence quality of material.
Material is after oven dry finishes, and the type of cooling that adopts at present is that nature dries, and needs 30-60min but dried in the air to the temperature of finished product packing by higher bake out temperature, length consuming time, and efficient is low, has a strong impact on production capacity.
Summary of the invention
The purpose of this invention is to provide a kind of HIGH-PURITY SILICON material drying unit, it is inhomogeneous to have solved in the prior art drying materials, dries length consuming time, inefficient technical problem.
Another object of the present invention provides a kind of method of utilizing above-mentioned device that the HIGH-PURITY SILICON material is dried, has solved in the prior art drying course, easily the material surface is polluted, and reduces feed purity, influences quality of material; Length consuming time has a strong impact on the problem of production capacity.
The technical scheme that the present invention adopted is, a kind of HIGH-PURITY SILICON material drying unit comprises casing,
Described casing is a kind of seal case with hermatic door, has vacuum orifice and vacuum checking hole on the wall box, and vacuum orifice is communicated with vacuum extractor, and vacuum checking hole is communicated with vacuum meter;
Also be provided with the outlet of heat-conducting medium import and heat-conducting medium on the sidewall of casing, heat-conducting medium import and heat-conducting medium outlet are communicated with the medium circulation heater;
Be provided with the drip pan support of the multilayer of connection in the inner chamber of casing; Neighbouring drip pan support is communicated with successively; Said drip pan support is a hollow tube; One end of drip pan support is communicated with the heat-conducting medium import, and the drip pan support other end is communicated with the heat-conducting medium outlet, is placed with one deck drip pan on every layer the drip pan support;
Vacuum extractor and medium circulation heater are connected with control device respectively.
Another technical scheme that the present invention adopted is that a kind of HIGH-PURITY SILICON material furnace drying method utilizes above-mentioned device, implements according to following steps:
Step 1. is put into drip pan with the different shape polycrystalline silicon material, then drip pan is placed on the drip pan support, closes hermatic door; Open valve K1 also connects vavuum pump; Begin to vacuumize, when the vacuum meter indication reaches 20-100Pa, first valve-off K1; Close vavuum pump again, be in vacuum state in the casing this moment;
Step 2. control device for opening, when the bright expression of indicator lamp is in proper working order, the temperature of instrument show case intracoelomic cavity; Set this temperature and be not less than 50 ℃, maximum temperature is set according to the character of heat-conducting medium, opens firing equipment; To the tank bottom heating, after the heat-conducting medium in the storage tank reaches design temperature, open the heat-conducting medium pump and give conveying heat-conducting medium in the casing; Drip pan support to box house heats, and promptly the polycrystalline silicon material in the drip pan is carried out heating, drying;
Behind the step 3. heating, drying 5-15min, open valve K2 and K3, simultaneously valve-off K1; Adopt moisture content detection device to monitor the drying effect of box house in real time; Detection range 0.01-1ppm, when showing the content requirement that arrives regulation, the polycrystalline silicon material drying course of expression box house finishes;
After step 4. oven dry finishes, close working power earlier, open the vacuum breaker butterfly valve in the pneumatic vacuum breaker mouth again,, remove the vacuum state of box house, open hermatic door then if pneumatic unlatching gets nowhere then opens manual vacuum breaker mouth, the taking-up polycrystalline silicon material.
The invention has the beneficial effects as follows:
1) apparatus structure among the present invention is simple, adopts conduction oil, steam or water as heat-conducting medium, and the silicon material places drip pan, be heated evenly, and good drying effect, energy consumption is little, and efficient is high.
2) HIGH-PURITY SILICON material that will be to be dried utilizes vavuum pump to be evacuated after being placed in the casing, reduces the vapourizing temperature of moisture, realizes oven dry through heating, and moisture content detection device is installed on vacuum lead, can detect drying effect in real time.
3) drying time is short.Vacuumized the vapourizing temperature of back reduction moisture in the casing, heat time heating time is short, and silicon material drying rate is fast.
4) cool time is short.Time in the casing is short, and vapourizing temperature is low, and on the box inside wall, also is provided with radiator coil tube, the silicon material rapid heat dissipation in the casing, and cool time is short.
Description of drawings
Fig. 1 is the front view of drying unit of the present invention;
Fig. 2 is the side view of drying unit of the present invention;
Fig. 3 is the internal view of drying unit of the present invention;
Fig. 4 is the moisture content detection device installation site sketch map in the drying unit of the present invention.
Among the figure, 1. casing, 2. vacuum meter, 3. lock valve, 4. manual vacuum breaker mouth; 5. base, 6. hermatic door, 7. vacuum orifice, 8. pneumatic vacuum breaker mouth, 9. vacuum checking hole; 10. temperature detecting resistance, 11. heat-conducting medium imports, the outlet of 12. heat-conducting mediums, 13. sewage draining exits, 14. drip pans; 15. the drip pan support, 16. radiator coil tubes, 17. vavuum pumps, 18. moisture content detection devices, 19. vacuum buffer tanks.
The specific embodiment
Below in conjunction with the accompanying drawing and the specific embodiment the present invention is elaborated.
With reference to Fig. 1, Fig. 2 and Fig. 3, the structure of apparatus of the present invention is, comprises casing 1, and casing 1 is connected with vacuum extractor and medium circulation heater through pipeline, and vacuum extractor and medium circulation heater are connected with the control device signal respectively;
Casing 1 is a kind of seal case with hermatic door 6, adopts corrosion-resistant, resistant to elevated temperatures stainless steel; Realizing being tightly connected through eight lock valves 3 between the main body of casing 1 and the hermatic door 6, (setting of lock valve 3 is each two groups of upper and lower, left and right; Every limit is installed two; Or the lock valve 3 of two above quantity is installed on every as required limit); Make hermatic door 6 and whole box body 1 inner chamber be in reliable closed state after fastening lock valve 3, can guarantee drying effect better;
The lower surface of casing 1 is provided with base 5, and the bottom of casing 1 has sewage draining exit 13, is used to discharge condensed water and cleaning sewage, on the pipeline of sewage draining exit 13 Vacuum ball valve is installed;
The sidewall of casing 1 is provided with two vacuum breaker mouths, is respectively manual vacuum breaker mouth 4 and pneumatic vacuum breaker mouth 8, manually is equipped with the vacuum breaker butterfly valve in vacuum breaker mouth 4 passages, is used for the external and internal pressure of balance box 1; Pneumatic vacuum breaker mouth 8 structures and effect are with manually vacuum breaker mouth 4 is consistent;
Also be provided with vacuum orifice 7, vacuum checking hole 9, heat-conducting medium import 11 and heat-conducting medium outlet 12 on the casing 1; Vacuum orifice 7 wherein is connected with the vavuum pump unit through the seamless stainless steel pipeline; Vacuum checking hole 9 is communicated with vacuum meter 2 through pipeline, and vacuum meter 2 is arranged on the outside of casing 1, and vacuum meter 2 can accurately show the vacuum of casing 1 inside;
With reference to Fig. 3; Be provided with the drip pan support 15 of multilayer in the inner chamber of casing 1; Neighbouring drip pan support 15 is communicated with successively, and said drip pan support (15) is a hollow tube, makes heat-conducting medium every layer of S-type flowing of drip pan support 15 inner chambers; Avoid thermal medium in drip pan support 15, to form short circuit and directly flow through, so just utilized the thermal source heat exchange fully; Drip pan support 15 bottom is communicated with heat-conducting medium import 11, and drip pan support 15 topmost is communicated with heat-conducting medium outlet 12.Radiator coil tube 16 is fixedly mounted on casing 1 inwall, and radiator coil tube 16 is close to drip pan support 15 and is used for heat radiation;
Every layer of drip pan support 15 is provided with rack rails, and rack rails is provided with drip pan 14.Every layer of drip pan support 15 realized that with drip pan 14 separately the engagement push-and-pull cooperates, and both can control automatically through the control system, and the push-and-pull speed during control is 0-0.2m/s, during shutdown, and manually push-and-pull again.
With reference to Fig. 4; Said vacuum extractor comprises vavuum pump 17, vacuum buffer tank 19 and moisture content detection device 18; Vavuum pump 17 adopts two or two above different model lobe pump series connection uses, can extract the gas that contains a large amount of steam, has certain corrosivity or coercibility; Vacuum buffer tank 19 is arranged on the pipeline between vavuum pump 17 and the vacuum orifice 7, can avoid vacuum extractor to shut down back recirculated water and pour in down a chimney into casing; The detection range of moisture content detection device 18 is 0.01-1ppm; Moisture content detection device 18 is arranged on the pipeline between vacuum buffer tank 19 and the vacuum orifice 7;,, when avoiding pouring in down a chimney this moisture content detection device 18 is damaged more near casing 1 than vacuum buffer tank 19; In addition, between vacuum orifice 7 and vacuum buffer tank 19, be provided with valve K1, between vacuum orifice 7 and moisture content detection device 18, be provided with valve K2, between moisture content detection device 18 and vacuum buffer tank 19, be provided with valve K3.
Said medium circulation heater comprises the storage tank that is arranged on outside the casing 1, stores heat-conducting medium in the storage tank, and heat-conducting medium is selected water, steam or conduction oil for use; The storage tank outer surface is enclosed with insulation material, realizes the insulation purpose; Storage tank is provided with heat-conducting medium delivery outlet, heat-conducting medium return port, heat-conducting medium circulating pump and pipeline; The heat-conducting medium delivery outlet is communicated with heat-conducting medium import 11 on the casing 1; Heat-conducting medium outlet 12 on heat-conducting medium return port and the casing 1 is communicated with; Heat-conducting medium is conveyed into the inner guiding pipe of drip pan support 15 through pipeline by heat-conducting medium import 11, S-typely progressively upwards flows, and is back to the storage tank recycle through heat-conducting medium outlet 12 again; Be provided with filter in the pipeline, be used for impurity screening; Be provided with firing equipment in tank bottom, the heat-conducting medium heating and temperature control in the storage tank is at 100 ℃-350 ℃.
Said control device comprises electric cabinet and temperature detecting resistance 10, and electric cabinet is wherein taked independent placement, and electric cabinet is provided with temperature control instrument and overtemperature alarm device, and this temperature control instrument is the control maincenter with the single-chip microcomputer, has digital PID and self-setting function; Temperature detecting resistance 10 is installed in the casing 1; The effect of temperature detecting resistance 10 is internal temperatures of test casing 1; And be connected through holding wire with electric cabinet; Electric cabinet in addition with firing equipment through the holding wire control connection, when the heating-up temperature casing 1 in surpassed 5 ℃ of design temperatures or conduction oil temperature and surpasses 2 ℃ of design temperatures, the overtemperature alarm device will start immediately reported to the police and the shutoff firing equipment stops to heat.
HIGH-PURITY SILICON material furnace drying method of the present invention utilizes above-mentioned device, implements according to following steps:
Step 1. is put into drip pan 14 with the different shape polycrystalline silicon material, is placed on then on the drip pan support 15, closes hermatic door 6; Open valve K1 also connects vavuum pump 17, begins to vacuumize, approximately behind the 2-5min; When vacuum meter 2 indications reach 20-100Pa; The valve-off K1 of elder generation closes vavuum pump 17 again, and be in vacuum state in the casing 1 this moment.
Step 2. control device for opening, when the bright expression of indicator lamp was in proper working order, instrument showed the temperature of casing 1 inner chamber; Set this temperature and be not less than 50 ℃, maximum temperature is set according to the character of heat-conducting medium, opens firing equipment; To the tank bottom heating, after the heat-conducting medium in the storage tank reaches design temperature, open the heat-conducting medium pump and give conveying heat-conducting medium in the casing 1; Casing 1 inner drip pan support 15 is heated, just the polycrystalline silicon material in the drip pan 14 is carried out heating, drying;
Behind the step 3. heating, drying 5-15min; Open valve K2 and K3, valve-off K1 adopts moisture content detection device 18 drying effect of monitoring casing 1 inside in real time simultaneously; When showing the content requirement that arrives regulation, expression casing 1 inner polycrystalline silicon material drying course finishes;
After step 4. oven dry finishes; Close working power earlier, open the vacuum breaker butterfly valve in the pneumatic vacuum breaker mouth 8, if pneumatic unlatching gets nowhere then opens manual vacuum breaker mouth 4; Remove the vacuum state of casing 1 inside; Lock valve 3 on the turn casing 1 is opened hermatic door 6 then, the taking-up polycrystalline silicon material.Polycrystalline silicon material after the oven dry can directly be packed.
As shown in Figure 4, the moisture content detection device workflow in the inventive method is, before the heating starting; Open valve K1, valve-off K2 and valve K3 are when treating that oven dry is near completion; Open valve K2 and valve K3, valve-off K1 observes moisture content detection device; If show moisture in HIGH-PURITY SILICON drying requirement scope, then show this drying course completion; If do not reach the regulation requirement, continue oven dry until meeting the requirements.
The oven dry principle of polycrystalline silicon material of the present invention is, the HIGH-PURITY SILICON material of oven dry is placed in the casing of sealing, uses vavuum pump to vacuumize; In 1-3min, vacuum promptly is stabilized in 20-100Pa, and the vapourizing temperature of moisture is reduced to 5-25 ℃; Realize oven dry through heating; And detect drying effect in real time, until meeting specification requirement.
Claims (10)
1. HIGH-PURITY SILICON material drying unit is characterized in that: comprise casing (1),
Described casing (1) is the seal case of a kind of band hermatic door (6), has vacuum orifice (7) and vacuum checking hole (9) on casing (1) sidewall, and vacuum orifice (7) is communicated with vacuum extractor, and vacuum checking hole (9) is communicated with vacuum meter (2);
Also be provided with heat-conducting medium import (11) and heat-conducting medium outlet (12) on the sidewall of casing (1), heat-conducting medium import (11) and heat-conducting medium outlet (12) are communicated with the medium circulation heater;
Be provided with the drip pan support (15) of the multilayer of connection in the inner chamber of casing (1); Neighbouring drip pan support (15) is communicated with successively; Said drip pan support (15) is a hollow tube; One end of drip pan support (15) is communicated with heat-conducting medium import (11), and drip pan support (15) other end is communicated with heat-conducting medium outlet (12), is placed with one deck drip pan (14) on every layer the drip pan support (15);
Vacuum extractor and medium circulation heater are connected with control device respectively.
2. HIGH-PURITY SILICON material drying unit according to claim 1 is characterized in that: described vacuum extractor comprises vavuum pump (17), vacuum buffer tank (19) and moisture content detection device (18),
Vacuum buffer tank (19) one ends are communicated with vacuum orifice (7), and vacuum buffer tank (19) other end is communicated with vavuum pump (17),
Pipeline between vacuum buffer tank (19) and the vacuum orifice (7) is provided with moisture content detection device (18),
Pipeline between vacuum orifice (7) and the vacuum buffer tank (19) is provided with valve K1,
Pipeline between vacuum orifice (7) and the moisture content detection device (18) is provided with valve K2,
Pipeline between moisture content detection device (18) and the vacuum buffer tank (19) is provided with valve K3.
3. HIGH-PURITY SILICON material drying unit according to claim 1; It is characterized in that: described medium circulation heater comprises the storage tank that is arranged on outside the casing (1); Store heat-conducting medium in the storage tank, the storage tank outer surface is enclosed with insulation material, is provided with firing equipment in tank bottom.
4. HIGH-PURITY SILICON material drying unit according to claim 1 is characterized in that: described control device comprises electric cabinet and temperature detecting resistance (10), and temperature detecting resistance (10) is arranged in the casing (1), and temperature detecting resistance (10) is connected with the electric cabinet signal.
5. according to claim 2,3 or 4 described HIGH-PURITY SILICON material drying units, it is characterized in that: the sidewall of described casing (1) has two vacuum breaker mouths, is respectively manual vacuum breaker mouth (4) and pneumatic vacuum breaker mouth (8).
6. according to claim 2,3 or 4 described HIGH-PURITY SILICON material drying units, it is characterized in that: described casing (1) madial wall is provided with radiator coil tube (16), radiator coil tube (16) and drip pan support (15) next-door neighbour.
7. according to claim 2,3 or 4 described HIGH-PURITY SILICON material drying units, it is characterized in that: be provided with rack rails between described every layer of drip pan support (15) and the corresponding drip pan (14).
8. according to claim 2,3 or 4 described HIGH-PURITY SILICON material drying units, it is characterized in that: the bottom of described casing (1) has sewage draining exit (13), and the lower surface of casing (1) is provided with base (5).
9. HIGH-PURITY SILICON material furnace drying method is characterized in that: utilize the described device of claim 2, implement according to following steps:
Step 1, the different shape polycrystalline silicon material is put into drip pan (14), then drip pan (14) is placed on the drip pan support (15), close hermatic door (6); Open valve K1 also connects vavuum pump (17); Begin to vacuumize, when vacuum meter (2) indication reaches 20-100Pa, first valve-off K1; Close vavuum pump (17) again, be in vacuum state in casing this moment (1);
Step 2, control device for opening, when the bright expression of indicator lamp was in proper working order, instrument showed the temperature of casing (1) inner chamber; Set this temperature and be not less than 50 ℃, maximum temperature is set according to the character of heat-conducting medium, opens firing equipment; Tank bottom is heated; After the heat-conducting medium in the storage tank reaches design temperature, open the heat-conducting medium pump, give and carry heat-conducting medium in the casing (1); Heat-conducting medium flows through each layer drip pan support (15), promptly the polycrystalline silicon material in the drip pan (14) is carried out heating, drying;
Behind step 3, the heating, drying 5-15min; Open valve K2 and K3; Valve-off K1 adopts moisture content detection device (18) to monitor the inner drying effect of casing (1), detection range 0.01-1ppm in real time; When showing the content requirement that arrives regulation, the inner polycrystalline silicon material drying course of expression casing (1) finishes;
After step 4, oven dry finish; Close working power earlier, open the vacuum breaker butterfly valve in the pneumatic vacuum breaker mouth (8) again, if pneumatic unlatching gets nowhere then opens manual vacuum breaker mouth (4); Remove the inner vacuum state of casing (1); Open hermatic door (6) then, take out polycrystalline silicon material.
10. HIGH-PURITY SILICON material furnace drying method according to claim 9; It is characterized in that: in the described step 2; Overtemperature alarm device in the described control device is set to; When the heating-up temperature in the casing (1) surpassed 5 ℃ of design temperatures or conduction oil temperature and surpasses 2 ℃ of design temperatures, starting immediately reports to the police and turn-off firing equipment stopped to heat.
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Cited By (8)
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| CN105333703A (en) * | 2015-12-14 | 2016-02-17 | 重庆正合印务有限公司 | Paperboard drying room |
| CN105352285A (en) * | 2015-12-14 | 2016-02-24 | 重庆正合印务有限公司 | Paperboard drying room |
| CN105352284A (en) * | 2015-12-14 | 2016-02-24 | 重庆正合印务有限公司 | Paperboard drying room |
| CN106482465A (en) * | 2016-12-15 | 2017-03-08 | 湖北科阳节能设备有限公司 | A kind of air-energy dryer being applied to Chinese herbal medicine |
| CN107462019A (en) * | 2017-09-25 | 2017-12-12 | 南京天煌机械有限公司 | One Room dual temperature vacuum drying chamber and furnace drying method |
| CN109059449A (en) * | 2018-08-30 | 2018-12-21 | 深圳市智创谷技术有限公司 | A kind of high vacuum dry device |
| CN109186103A (en) * | 2018-07-10 | 2019-01-11 | 上海理工大学 | Solar thermal collector heat preservation utilizes and residual heat drying integrated apparatus |
| CN109387041A (en) * | 2018-11-26 | 2019-02-26 | 山东农业大学 | Multifunctional food is dried in vacuo curer |
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| CN109387041A (en) * | 2018-11-26 | 2019-02-26 | 山东农业大学 | Multifunctional food is dried in vacuo curer |
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| CN102818439B (en) | 2015-01-14 |
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Address after: 710100 Changan District, Shaanxi Province, aerospace Road, No. 388, No. Co-patentee after: Wuxi LONGi Silicon Materials Corp. Patentee after: Longji green energy Polytron Technologies Inc Co-patentee after: Ningxia LONGi Silicon Material Co.,Ltd. Co-patentee after: Yinchuan LONGi Silicon Material Co.,Ltd. Address before: 710100 Changan District, Shaanxi Province, aerospace Road, No. 388, No. Co-patentee before: Wuxi LONGi Silicon Materials Corp. Patentee before: Xi'an Longji-Silicon Co., LTD. Co-patentee before: Ningxia LONGi Silicon Material Co.,Ltd. Co-patentee before: Yinchuan LONGi Silicon Material Co.,Ltd. |
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Effective date of registration: 20211012 Address after: 710199 no.388 Hangtian Middle Road, Chang'an District, Xi'an City, Shaanxi Province Patentee after: LONGI GREEN ENERGY TECHNOLOGY Co.,Ltd. Address before: 710100 No. 388, middle route, Xi'an, Shaanxi, Changan District Patentee before: LONGI GREEN ENERGY TECHNOLOGY Co.,Ltd. Patentee before: WUXI LONGI SILICON MATERIALS Corp. Patentee before: NINGXIA LONGI SILICON MATERIALS Co.,Ltd. Patentee before: YINCHUAN LONGI SILICON MATERIALS Co.,Ltd. |