CN206404534U - The multilayer adsorption tower purified for electronic-grade polycrystalline silicon tail gas - Google Patents
The multilayer adsorption tower purified for electronic-grade polycrystalline silicon tail gas Download PDFInfo
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- CN206404534U CN206404534U CN201621453271.3U CN201621453271U CN206404534U CN 206404534 U CN206404534 U CN 206404534U CN 201621453271 U CN201621453271 U CN 201621453271U CN 206404534 U CN206404534 U CN 206404534U
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Abstract
The utility model discloses a kind of multilayer adsorption tower purified for electronic-grade polycrystalline silicon tail gas, a kind of multilayer adsorption tower purified for electronic-grade polycrystalline silicon tail gas, if tower body is divided into several tower rooms by dried layer column plate, tower top is provided with gas inlet pipe provided with gas outlet tube and bottom of towe；Hollow outer coil pipe is wound with outside the tower body, the two ends of the outer coil pipe are provided with outer coil inlet and outer coil outlets.Sorbing material is filled with the tower room, polytype sorbing material is filled with different tower rooms, such as molecular sieve, the activated carbon of different pore size, the efficiency for hydrogen purification can be effectively improved using multilayer adsorption tower of the present utility model purifying electronic-grade polycrystalline silicon tail gas, and the hydrogen of the high-purity to obtain can produce the integrated circuit grade multi-crystalline silicon of higher purity as raw material.
Description
Technical field
The utility model is related to boron, the phosphorus that electronic-grade polycrystalline silicon production field, particularly improved Siemens reclaim hydrogen
The removal of element impurity.
Background technology
In existing improved Siemens production of polysilicon technology, tail gas recycle mainly uses Dry recovery.Hydrogen, chlorosilane
The mixture constituted with hydrogen chloride eluted by low temperature, the process such as absorb is separated, contain a small amount of chlorosilane, hydrogen chloride and
The hydrogen of other impurities leads to adsorption tower, is purified in adsorption tower using activated carbon.
Generally all adsorbed in current adsorption tower using single adsorption material, and chlorosilane, chlorination are contained in hydrogen
Hydrogen, BCl3、PCl3And the impurity of other unknown compositions, the adsorption tower of single adsorption material can not be pure to hydrogen progress well
Change.
Electronic-grade polycrystalline silicon is produced, in the production especially for integrated circuit with semiconductor grade high purity polycrystalline silicon, each original
The control of material need to be very strict, and the purity that the impurity for bringing reduction furnace into by hydrogen will result directly in polysilicon product is not enough.
For example in the prior art generally using cocoanut active charcoal as sorbing material, although cocoanut active charcoal possesses many excellent
Point, but based on material self character, its hole is essentially micropore, i.e. aperture less than 2nm, and some impurity profit contained in hydrogen
It is not good with micro-porous adsorption effect, and can therefore cause part important goal impurity such as B, P adsorption effect.
Utility model content
The technical problems to be solved in the utility model is：A kind of multilayer suction purified for electronic-grade polycrystalline silicon tail gas is provided
Adsorption device and its application method, realize the target of steady production electronic-grade polycrystalline silicon.
A kind of multilayer adsorption tower purified for electronic-grade polycrystalline silicon tail gas, if tower body is divided into several by dried layer column plate
Tower room, tower top is provided with gas inlet pipe provided with gas outlet tube and bottom of towe；Hollow outer coil pipe is wound with outside the tower body, it is described
The two ends of outer coil pipe are provided with outer coil inlet and outer coil outlets.
It is preferred that, tower body is built-in with hollow inner cylinder, and the hollow inner cylinder runs through tower room up to close tower top position from bottom of towe,
The hollow inner cylinder bottom is provided with outer extension, and the outer extension is passed outside tower by the hole of bottom of towe, and the hollow inner cylinder is set
There are inner cylinder outlet and inner cylinder inlet tube, the inner cylinder outlet is located at the bottom of the hollow inner cylinder, the inner cylinder inlet tube
Extended to from the bottom of the hollow inner cylinder outside top, the hollow inner cylinder and be wound with hollow inner coil pipe, the inner coil pipe
Two ends exported provided with inner disc tube inlet and inner coil pipe, inner disc tube inlet and the inner coil pipe outlet passes tower body.
The tower room can be with multiple, preferably 2~6, each independent in the tower room to be filled with sorbing material.Often
The bottom plate of one floor tower room is dismountable, and sorbing material landfill is on bottom plate.Install and fill out in layer from the bottom up during installation
Fill.
The tower room can be 4, and the sorbing material is independently selected from molecular sieve, No. 1 activated carbon, No. 2 activity
Charcoal and No. 3 activated carbons, No. 1 activated carbon are cocoanut active charcoal, and described No. 2 and No. 3 activated carbons are coal mass active carbon.
The aperture of the molecular sieve is 0.3-1nm；No. 1 activated carbon is cocoanut active charcoal, and its primary aperture is less than
2nm, correspondence pore volume is 3-6ml/g；No. 2 activated carbons are coal mass active carbon, and its primary aperture is 2-50nm, and correspondence pore volume is
1-3ml/g；No. 3 activated carbons are coal mass active carbon, and its primary aperture is more than 50nm, and correspondence pore volume is 0.5-2ml/g.
A kind of method for purifying electronic-grade polycrystalline silicon tail gas using any of the above-described multilayer adsorption tower：
When needing purifying hydrogen, by the circulating hydrogen that need to be purified by heat exchanger be cooled to -20 to 0 DEG C between after, from institute
State gas inlet pipe and be passed through multilayer adsorption tower and go the removal of impurity, it is 0.5~2 atmospheric pressure to control the pressure of adsorption tower, is purified
Hydrogen afterwards is passed through electronic-grade polycrystalline silicon production system from the gas outlet tube.
When needing to regenerate the sorbing material in the adsorption tower, at least one into the inner coil pipe, outer coil pipe or inner cylinder
The adsorption tower is warming up to 150~200 DEG C by the individual thermal medium that is passed through, and it is 0.5~2 atmospheric pressure to control the pressure of adsorption tower, from
The hydrogen outlet blowback enters pure hydrogen, and sorbing material in adsorption tower is regenerated.
It is preferred that inner coil pipe, outer coil pipe or inner cylinder in be all passed through thermal medium heating.
A kind of system of tail gas purifying, includes any described multilayer adsorption tower of the utility model.
Have above in the middle of three heating regions, outer coil pipe heat external region, inner cylinder heating interior zone, inner coil pipe heating
Region.It is preferred that three regions heat simultaneously, reach optimal addition effect.
Sorbing material described in the utility model be in porous media, such Porous Medium Adsorption hydrogen impurity it is main according to
By its different size of micropore, if aperture is much larger than molecular motion diameter, absorption is not susceptible to, if aperture is transported slightly larger than molecule
Dynamic diameter, then occur firm absorption, but regeneration is difficult, if aperture is less than molecular motion diameter, is not adsorbed.In the past
Often aperture concentrates on below 2nm to general activated carbon, and not only absorption total capacity is not good, and can form competitive Adsorption, influences
The absorption of common-denominator target material.The characteristics of for the above, the utility model takes into account the convenience of adsorbing medium regeneration, selection simultaneously
The porous media of above-mentioned different pore size is sorbing material.The sorbing material puts in order with main effective pore sife distribution
Size is standard.The utility model has preferably selected molecular sieve, cocoanut active charcoal, the mode pair of coal mass active carbon integrated use
Hydrogen carries out adsorption-edulcoration.The sorbing material of this 4 characteristics carries out one that many heavily adsorbs can be in more effective adsorbed hydrogen
Serial impurity, the impurity that each layer of adsorbent is all removed for different need has stronger adsorption capacity, wherein, the molecule
Sieve is directed to O2, N2, BH3, PH3；No. 1 activated carbon is directed to CH4, CO2, HCL, BCL3, PCL3, and No. 2 activated carbons are directed to
Trichlorosilane, dichlorosilane, silicon tetrachloride；No. 3 activated carbons are mainly used in the absorption of silicon hexachloride, polysilane.
Pore volume denotes total adsorption capacity of adsorbing medium, because total pore volume difference is less, and corresponding pore volume can certain journey
Reflect the Pore Characteristics of adsorbing medium on degree, so being used as the secondary finger of adsorbing medium performance using the corresponding pore volume of primary aperture
Mark.
After adsorption operations after a while, regenerative operation is carried out, in whole production process, absorption and regeneration can be with
Constantly repeat.
Traditional theory thinks, the impurity contained in coal mass active carbon is unfavorable for electronic-grade polycrystalline silicon system, but this reality
Shown with new actual effect, coal mass active carbon will not separate out B, P etc. because performance is stable in gas adsorption processes
Impurity.Due in hydrogen B the impurity content such as P it is extremely micro, it is impossible to directly with apparatus measures, we are with the electricity of finished product polysilicon
Resistance rate and minority carrier life time are compared, and are found using multilayer of the present utility model absorption relative to traditional individual layer cocoanut active charcoal
Absorption, clearly, the resistivity and minority carrier life time of the utility model finished product polysilicon are all much improved improvement.
Beneficial effect：The efficiency for hydrogen purification can be effectively improved using multilayer adsorption tower of the present utility model, and
The hydrogen of high-purity to obtain can produce the integrated circuit grade multi-crystalline silicon of higher purity as raw material.
Brief description of the drawings
Fig. 1 is profile of the present utility model, wherein 1~4 is respectively 1~4 tower room；5 be gas inlet pipe, and 6 be gas
Outlet, 7 be hollow inner cylinder, and 701 be inner cylinder inlet tube, and 702 be inner cylinder outlet, and 703 be the outer extension of inner cylinder, and 8 be inner disc
Pipe, 801 be inner disc tube inlet, and 802 be inner coil pipe outlet, and 9 be outer coil pipe, and 901 be outer coil inlet, and 902 be that outer coil pipe goes out
Mouthful.
Embodiment
According to following embodiments, the utility model may be better understood.However, those skilled in the art easily manages
Solution, the content described by embodiment is merely to illustrate the utility model, without should also without limitation on institute in claims in detail
The utility model carefully described.
Embodiment 1
It is a kind of for electronic-grade polycrystalline silicon tail gas purify multilayer adsorption tower, if including tower body and column plate dried layer, tower body lead to
Cross 3 floor column plate and be divided into 4 tower rooms, bottom of towe is provided with gas inlet pipe 5, and tower top is provided with gas outlet tube 6；Tower body is built-in with hollow
Inner cylinder 7, the hollow inner cylinder 7 is from bottom of towe through tower room until close to tower top position, the bottom of the hollow inner cylinder 7 is provided with extension
Section 703 is stretched, the outer extension 703 is passed outside tower by the hole of bottom of towe, the hollow inner cylinder 7 is provided with the He of inner cylinder inlet tube 701
Inner cylinder outlet 702, the inner cylinder outlet 701 is located at the bottom of the hollow inner cylinder 7, and the inner cylinder inlet tube 701 is from institute
The bottom for stating hollow inner cylinder extends to top, is wound with hollow inner coil pipe 8, the two of the inner coil pipe outside the hollow inner cylinder
End passes tower body provided with inner disc tube inlet 801 and inner coil pipe outlet 802, inner disc tube inlet 801 and the inner coil pipe outlet 802,
Hollow outer coil pipe 9 is wound with outside the tower body, the two ends of the outer coil pipe are provided with outer coil inlet 901 and outer coil outlets
902。
Chlorosilane, hydrogen chloride, BCl will be contained3、PCl3And the hydrogen of other plurality of impurities is cooled to -10 by heat exchanger
DEG C, adsorption tower is passed through from 5 mouthfuls of tower bottom of absorption, absorption tower pressure interior force maintains 1 atmospheric pressure, and hydrogen is adsorbed by 4 floor tower rooms
Afterwards, most impurity are adsorbed, and high-purity hydrogen is drawn for 6 mouthfuls from tower top.After continuous operation in 8 hours, adsorption effect meeting
Start to have declined, now need to enter step for regeneration.First stop being passed through the hydrogen that need to purify, in coil pipe built in adsorption tower, interior
Conduction oil being passed through in cylinder, outer coil pipe adsorption tower is warming up to after 180 DEG C, blowback hydrogen being passed through from top, pressure is 2 air
Pressure, the impurities purging that sorbing material in adsorption tower is adsorbed comes out, and tail gas leads to exhaust gas processing device, and the regenerative process continues
4 hours.After the completion of regenerative process, in built-in coil pipe, inner cylinder, outer coil pipe be passed through glycol water cools to system,
Through after a period of time, adsorption tower temperature is down to -10 DEG C and stablized after 10~30 minutes, you can carry out adsorption process again.
In whole production process, absorption and regeneration constantly repeat.Generally whole system is equipped with 3 adsorption towers simultaneously
Connection, maintains 1 adsorption tower and is in adsorbed state all the time.
Table 1 is that the effect that conventional dry is reclaimed between hydrogen and the utility model method multilayer adsorption recovery hydrogen compares,
The impurity in hydrogen is detected using gas chromatograph.
The effect that the conventional dry of table 1 is reclaimed between hydrogen and the utility model method multilayer adsorption recovery hydrogen compares
The hydrogen reclaimed with the utility model reclaims the resistivity of finished product polysilicon prepared by hydrogen with conventional dry and lacked
Sub- life-span comparative result such as table 2, it is seen that improvement is clearly.
Claims (8)
1. a kind of multilayer adsorption tower purified for electronic-grade polycrystalline silicon tail gas, it is characterised in that if tower body passes through dried layer column plate
It is divided into several tower rooms, tower top is provided with gas inlet pipe provided with gas outlet tube and bottom of towe；It is wound with outside the tower body hollow
Outer coil pipe, the two ends of the outer coil pipe are provided with outer coil inlet and outer coil outlets.
2. the multilayer adsorption tower according to claim 1 purified for electronic-grade polycrystalline silicon tail gas, it is characterised in that described
Tower body is built-in with hollow inner cylinder, and the hollow inner cylinder is from bottom of towe through tower room until under tower top position, the hollow inner cylinder
Portion is provided with outer extension, and the outer extension passed outside tower by the hole of bottom of towe, the hollow inner cylinder provided with inner cylinder outlet and
Inner cylinder inlet tube, the inner cylinder outlet is located at the bottom of the hollow inner cylinder, and the inner cylinder inlet tube is from the hollow inner cylinder
Bottom extend to top, hollow inner coil pipe is wound with outside the hollow inner cylinder, the two ends of the inner coil pipe are provided with inner disc
Tube inlet and inner coil pipe outlet, inner disc tube inlet and the inner coil pipe outlet pass tower body.
3. the multilayer adsorption tower according to claim 1 purified for electronic-grade polycrystalline silicon tail gas, it is characterised in that described
Tower room is 2~6, each independent in the tower room to be filled with sorbing material.
4. the multilayer adsorption tower according to claim 3 purified for electronic-grade polycrystalline silicon tail gas, it is characterised in that described
Tower room is 4, and the sorbing material is independently selected from molecular sieve, No. 1 activated carbon, No. 2 activated carbons and No. 3 activated carbons, institute
It is cocoanut active charcoal to state No. 1 activated carbon, and described No. 2 and No. 3 activated carbons are coal mass active carbon.
5. the multilayer adsorption tower according to claim 4 purified for electronic-grade polycrystalline silicon tail gas, it is characterised in that described
The aperture of molecular sieve is 0.3-1nm, and the primary aperture of the cocoanut active charcoal is less than 2nm, and pore volume is 3-6ml/g.
6. the multilayer adsorption tower according to claim 4 purified for electronic-grade polycrystalline silicon tail gas, it is characterised in that described
The primary aperture of No. 2 activated carbons is 2-50nm, and pore volume is 1-3ml/g；The primary aperture of No. 3 activated carbons is more than 50nm, hole
Hold for 0.5-2ml/g.
7. the multilayer adsorption tower according to claim 3 purified for electronic-grade polycrystalline silicon tail gas, it is characterised in that described
Sorbing material is placed in tower room from top to bottom according to the order of primary aperture from small to large.
8. a kind of system of tail gas purifying, it is characterized in that including any described multilayer adsorption tower of claim 1~7.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621453271.3U CN206404534U (en) | 2016-12-28 | 2016-12-28 | The multilayer adsorption tower purified for electronic-grade polycrystalline silicon tail gas |
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|---|---|---|---|
| CN201621453271.3U CN206404534U (en) | 2016-12-28 | 2016-12-28 | The multilayer adsorption tower purified for electronic-grade polycrystalline silicon tail gas |
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| CN206404534U true CN206404534U (en) | 2017-08-15 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106512644A (en) * | 2016-12-28 | 2017-03-22 | 江苏鑫华半导体材料科技有限公司 | Multi-layer adsorption tower for purifying electronic grade polycrystalline silicon tail gas |
| CN113929054A (en) * | 2021-11-18 | 2022-01-14 | 无锡碳谷科技有限公司 | Hydrogen recovery device of methane catalytic cracking instrument |
-
2016
- 2016-12-28 CN CN201621453271.3U patent/CN206404534U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106512644A (en) * | 2016-12-28 | 2017-03-22 | 江苏鑫华半导体材料科技有限公司 | Multi-layer adsorption tower for purifying electronic grade polycrystalline silicon tail gas |
| CN113929054A (en) * | 2021-11-18 | 2022-01-14 | 无锡碳谷科技有限公司 | Hydrogen recovery device of methane catalytic cracking instrument |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 221004 No.66, Xiexin Avenue, Xuzhou Economic and Technological Development Zone, Jiangsu Province Patentee after: Jiangsu Xinhua Semiconductor Technology Co.,Ltd. Address before: 221004 No.66, Xiexin Avenue, Xuzhou Economic and Technological Development Zone, Jiangsu Province Patentee before: JIANGSU XINHUA SEMICONDUCTOR MATERIALS TECHNOLOGY CO.,LTD. |
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