CN101357292A - Method for recovering tail-gas generated during producing polycrystalline silicon using silicon tetrachloride - Google Patents
Method for recovering tail-gas generated during producing polycrystalline silicon using silicon tetrachloride Download PDFInfo
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- CN101357292A CN101357292A CNA2007101197445A CN200710119744A CN101357292A CN 101357292 A CN101357292 A CN 101357292A CN A2007101197445 A CNA2007101197445 A CN A2007101197445A CN 200710119744 A CN200710119744 A CN 200710119744A CN 101357292 A CN101357292 A CN 101357292A
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Abstract
A method for recovering tail gas produced in the process of polysilicon production by tetrachlorosilane comprises the following steps: the tail gas is leached by liquid tetrachlorosilane; the leached tail gas is pressurized and cooled; and hydrogen is separated from hydrogen chloride and dichlordihydrosilicate by an absorbent; the separated hydrogen is absorbed and filtrated by an absorbent, the hydrogen can be recovered; the hydrogen chloride and chlorosilane in the absorbent are heated, the gaseous hydrogen chloride and the gaseous chlorosilane are taken out by the hydrogen, and then the tail gas is recycled; the liquid tetrachlorosilane is heated and/or pressurized, therefore, the hydrogen chloride and the dichlordihydrosilicate are desorbed; and the hydrogen chloride and/or the dichlordihydrosilicate are recovered by gas-liquid separation. By adopting a dry method, the tail gas treated by the method can be reused in the polysilicon production, therefore, the method has the advantages of adequate utilization of raw materials, reducing pollutants, solving the problem of environmental pollution, improving product quality and lowering cost.
Description
Technical field
The present invention relates to the recovery and treatment method of the tail gas that a kind of industrial production polysilicon produced, more specifically, relate to a kind of silicon tetrachloride that utilizes producing the method that tail gas that polysilicon produced reclaims.
Background technology
Polysilicon is the raw material of preparation monocrystalline silicon, finally is used to produce integrated circuit and electronic device, and be one of the highest basic material of information industry consumption maximum, purity requirement, also be the product and the industry of state key encourage growth.
World advanced person's production of polysilicon technology by the company monopolizing of beautiful, day, moral three states always, all there be know-how and technical characterstic separately in each company, through constantly research, exploitation, formed production technology separately, and from national strategy angle separately, strict control technology transfer also monopolizes global polysilicon market.
China's polysilicon industry is started in the fifties, middle nineteen sixties is realized industrialization, early seventies is pell-mell development once, factory is family surplus in the of 20 nearly, and what all adopt is traditional Siemens process, backward in technique, environmental pollution is serious, supplies consumption is big, production cost height, most losses of enterprise and stop production in succession or change the line of production.
The outstanding characteristics of tradition production of polysilicon technology are tail gas hydrometallurgic recovery technology, be that tail gas in the reduction furnace is used water wash after preliminary pressurization separates chlorosilane, recover hydrogen, because in the water wash process, foreign gases such as water oxygen gas, carbon dioxide can be polluted hydrogen, so a large amount of hydrogen that reclaims needs to purify once more, chlorosilane hydrolysis in the lessivation, produce sewage, need further to handle, cause environmental pollution and supplies consumption big.Simultaneously, the hydrogen that produces in the production also fails to be fully utilized, and has both wasted the energy, has caused environmental pollution again.
Summary of the invention
Purpose of the present invention is intended to overcome at least one above-mentioned shortcoming of the prior art, a kind of method of utilizing silicon tetrachloride that the production tail gas that polysilicon produced is reclaimed is proposed, the method according to this invention utilizes dry method from tail gas recycle hydrogen, hydrogen chloride, dichloro-dihydro silicon and recycling silicon tetrachloride, therefore also can be called " tail gas dry process recovery " technology.
Utilize method of the present invention, not only can reclaim fully and silicon tetrachloride recycling, and can significantly reduce the generation of pollutant in the production, made full use of material simultaneously, reduced cost the hydrogen in the tail gas, hydrogen chloride, dichloro-dihydro silicon.
For achieving the above object, embodiments of the invention propose a kind of method of utilizing silicon tetrachloride that the production tail gas that polysilicon produced is reclaimed, described tail gas mainly comprises hydrogen, hydrogen chloride and chlorosilane, described chlorosilane mainly comprises dichloro-dihydro silicon, trichlorosilane and silicon tetrachloride, said method comprising the steps of: tail gas is carried out drip washing, the impurity in the tail gas of place to go and the hydrogen chloride of absorption portion and chlorosilane with liquid silicon tetrachloride; Tail gas after the drip washing is pressurizeed and cools off, described hydrogen, hydrogen chloride, dichloro-dihydro silicon remain gaseous state, thereby separate with silicon tetrachloride with the trichlorosilane of liquid state by hydrogen, hydrogen chloride and the dichloro-dihydro silicon of gas-liquid separation with gaseous state so that make described trichlorosilane and silicon tetrachloride become liquid; The hydrogen, hydrogen chloride and the dichloro-dihydro silicon that make gaseous state, so that the hydrogen chloride of gaseous state and dichloro-dihydro silicon are dissolved in the liquid silicon tetrachloride thereby separate with hydrogen chloride hydrogen by liquid silicon tetrachloride with dichloro-dihydro silicon; Utilize gaseous hydrogen chloride and chlorosilane remaining in adsorbents adsorb and the filtering hydrogen, thereby hydrogen is separated with chlorosilane with the hydrogen chloride of described remnants, thus recover hydrogen; Hydrogen chloride and the chlorosilane that is attracted in the adsorbent heated, and utilize gaseous hydrogen chloride and chlorosilane after hydrogen will heat in adsorbent, to take out of and turn back to the tail gas; The liquid silicon tetrachloride that has dissolved hydrogen chloride and dichloro-dihydro silicon is heated up and/or pressurizes, hydrogen chloride and dichloro-dihydro silicon are desorbed from stripping liquid; Make dichloro-dihydro silicon become liquid state with the hydrogen chloride of the gaseous state that desorbs by control and the pressure and/or the temperature of dichloro-dihydro silicon, thereby separating hydrogen chloride and dichloro-dihydro silicon reclaim hydrogen chloride and/or dichloro-dihydro silicon thus.
The further embodiment according to the present invention, described tail gas through drip washing is pressurized to 0.3～0.9Mpa.Described leacheate silicon tetrachloride is cooled to 20～-70 ℃.Described adsorbent is an active carbon.
The further embodiment according to the present invention, described from produce the tail gas that polysilicon produced the method for recover hydrogen comprise that also the silicon tetrachloride with liquid state carries out drip washing to tail gas.
More specifically, before to tail gas pressurization and cooling, tail gas is carried out drip washing.
Particularly, hydrogen chloride and the chlorosilane that is attracted in the adsorbent is heated to 80～220 ℃.
In addition, the gaseous hydrogen chloride that will be taken out of by hydrogen and silicon tetrachloride turn back in the middle of the tail gas, so that the circulation recover hydrogen.
The further embodiment according to the present invention, utilize silicon tetrachloride that the method that the production tail gas that polysilicon produced reclaims is also comprised:
To drip washing the liquid silicon tetrachloride of tail gas heat up and/or pressurize, the hydrogen chloride and the dichloro-dihydro silicon that are dissolved in the liquid silicon tetrachloride are desorbed from stripping liquid.
Wherein the hydrogen chloride of the gaseous state that desorbs by control and the pressure and/or the temperature of dichloro-dihydro silicon make dichloro-dihydro silicon become liquid state, thereby separating hydrogen chloride and dichloro-dihydro silicon reclaim hydrogen chloride and/or dichloro-dihydro silicon thus.
The temperature of the hydrogen chloride of the gaseous state that wherein desorbs particularly, and dichloro-dihydro silicon is controlled to be 30～-70 ℃.The pressure of the hydrogen chloride of the gaseous state that desorbs and dichloro-dihydro silicon is controlled to be 0.1～2.0Mpa.
According to the present invention, owing to adopt the tail gas that produces in the dry process production of polysilicon, therefore, overcome and eliminated the shortcoming of conventional wet recovery technology, hydrogen, hydrogen chloride, dichloro-dihydro silicon and silicon tetrachloride etc. in the tail gas are recycled simultaneously, especially it is turned back in the production of polysilicon operation, make the means of production can be able to sufficient utilization, and significantly reduced the generation and the quantity of pollutant in the production.
According to the present invention, material is in closed cycle is used, greatly reduce the consumption of raw and auxiliary material, fundamentally solved the problem of environmental pollution that production of polysilicon causes, simultaneously, save project investment, improved product quality, reduce cost, made the construction and upgrading of production of polysilicon project obtain sufficient initiative.
The feature and advantage that the present invention adds part in the following description provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Description of drawings
Fig. 1 is the industrial production schematic flow sheet of polysilicon;
Fig. 2 is the schematic flow sheet according to first embodiment of the invention.
The specific embodiment
So that explain the present invention, described embodiment is exemplary, can not be interpreted as limitation of the present invention below by describing specific embodiment with reference to the accompanying drawings.
Embodiment 1:
With reference to figure 1, wherein show to use and utilize the FB(flow block) of silicon tetrachloride the industrial production polysilicon of the method for producing tail gas that polysilicon produced and reclaiming according to the embodiment of the invention, in the prior art, there is several different methods can carry out the production of industrialization polysilicon, use production of polysilicon technology of the present invention, be that to utilize industrial silicon and hydrogen chloride (HCl) be primary raw material, generate with trichlorosilane (SiHCl by the control reaction condition
3) be master's the chlorosilane and the mixture of hydrogen, pass through existing purification technique then to trichlorosilane (SiHCl
3) purify after, send into reduction furnace, make trichlorosilane (SiHCl
3) and auxiliary material hydrogen (H
2) reaction, reduction generates polysilicon.
In the process of above-mentioned industrial production polysilicon, the tail gas of generation mainly comprises hydrogen (H
2), hydrogen chloride (HCl) and chlorosilane, described chlorosilane mainly comprises dichloro-dihydro silicon (SiH
2Cl
2), trichlorosilane (SiHCl
3) and silicon tetrachloride (SiCl
4).
Reaction main in the production process is:
Si+HCl→SiHCl
3+SiCl
4+H
2
SiHCl
3→Si+SiCl
4+H
2
SiHCl
3+H
2→Si+HCl
Need to prove, owing in primary industry silicon, also have plurality of impurities, for example iron, aluminium, boron, calcium or the like, so, in reaction, also can produce the chloride of calcium, the chloride of iron, the chloride of aluminium and the chloride of boron, and solid and/or gaseous impurities such as other high chlorosilanes, these impurity also can be mixed in the middle of the tail gas, certainly content is less, and the method according to this invention also can be handled these impurity, and this will be described below.
Below with reference to Fig. 2 describe according to first embodiment of the invention utilize silicon tetrachloride to producing the method that tail gas that polysilicon produced reclaims, Fig. 2 shows and utilizes the flow chart of silicon tetrachloride to the method for producing tail gas that polysilicon produced and reclaiming.
At first, the tail gas that produces in the polysilicon production process is collected, and tail gas is carried out drip washing, the impurity in the tail gas of place to go and the hydrogen chloride of absorption portion and chlorosilane with liquid silicon tetrachloride;
In the middle of traditional wet method tail gas treatment process process, usually all be that water carries out drip washing to tail gas, purpose is that the hydrogen chloride (HCl) in the tail gas is entered in the water by drip washing, the chlorosilane that part does not reclaim is hydrogen chloride and Silicon dioxide, hydrate by the water wash posthydrolysis, this type of sewage needs to handle separately, cause supplies consumption big, environmental pollution is serious, has limited large-scale industrialized production.
According to embodiments of the invention, lessivation adopts liquid silicon tetrachloride (SiCl
4), the effect and the effect of carrying out drip washing with traditional water are all inequality.In the present invention, adopt liquid silicon tetrachloride (SiCl
4) tail gas is carried out drip washing can remove impurity in the tail gas, as mentioned above, described tail gas is except mainly comprising hydrogen (H
2), hydrogen chloride (HCl), dichloro-dihydro silicon (SiH
2Cl
2), trichlorosilane (SiHCl
3) and silicon tetrachloride (SiCl
4), owing to produce in the process of polysilicon, also can produce impurity such as solid impurity and high chlorosilane, therefore, utilize liquid silicon tetrachloride (SiCl
4) tail gas is carried out drip washing, can remove the above-mentioned impurity in the tail gas.
In addition, owing in the production reduction process of polysilicon, also can produce the part accessory substance---silicon tetrachloride (SiCl
4), common every production 1kg polysilicon can produce the silicon tetrachloride (SiCl about 10kg
4), therefore, if silicon tetrachloride can't be handled and use, restriction is just received in the production of so much crystal silicon.
Therefore, according to the present invention, the silicon tetrachloride that produces in the production of polysilicon can be used for tail gas is carried out drip washing, on the other hand, adopts hydrogenation technology (reduction by hydrogen makes the silicon tetrachloride reaction produce trichlorosilane) silicon tetrachloride can be converted into trichlorosilane (SiHCl again
3), trichlorosilane (SiHCl
3) after purifying, can return in the production system again and reuse, thereby it is recycling that material is obtained in production of polysilicon.
Tail gas after the drip washing is pressurizeed and cools off, and for example, tail gas is pressurized to about 0.3～0.9Mpa and is cooled to about 20～-70 ℃, because described trichlorosilane (SiHCl
3) and silicon tetrachloride (SiCl
4) and described hydrogen (H
2), hydrogen chloride (HCl), dichloro-dihydro silicon (SiH
2Cl
2) between the boiling point difference, therefore, under above-mentioned process conditions, the trichlorosilane (SiHCl in the tail gas
3) and silicon tetrachloride (SiCl
4) become liquid state, and described hydrogen (H
2) still remain gaseous state, described hydrogen chloride (HCl) and dichloro-dihydro silicon (SiH simultaneously
2Cl
2) also mainly exist with gaseous form, thereby just hydrogen, hydrogen chloride and the dichloro-dihydro silicon of gaseous state can be separated with silicon tetrachloride with the trichlorosilane of liquid state by gas-liquid separation.
Above-mentioned pressure condition 0.3～0.9Mpa and temperature conditions 20～-70 ℃ only are exemplary, for those having ordinary skill in the art will appreciate that, as long as can separate with silicon tetrachloride with the trichlorosilane of liquid state by hydrogen, hydrogen chloride and the dichloro-dihydro silicon of gas-liquid separation with gaseous state, any suitable pressure and temperature condition can be used.
Then, utilize liquid silicon tetrachloride (SiCl
4) as absorbent, make the hydrogen chloride (HCl) and the dichloro-dihydro silicon (SiH of gaseous state
2Cl
2) be dissolved in the absorbent, so that with the hydrogen (H of gaseous state
2) and hydrogen chloride (HCl) and dichloro-dihydro silicon (SiH
2Cl
2) initial gross separation, yet, for persons of ordinary skill in the art may appreciate that in isolated gaseous hydrogen, still have the gaseous hydrogen chloride (HCl) and the silicon tetrachloride (SiCl of small portion of residual
4) be mixed in wherein.In addition, need to prove that absorbent is not limited to liquid silicon tetrachloride.
At last, utilize adsorbent that hydrogen is adsorbed and filter, so that absorption and filtering hydrogen (H
2) in a small amount of remaining gaseous hydrogen chloride (HCl) that is mixed with and chlorosilane (here, described chlorosilane main component is silicon tetrachloride (SiCl
4)), thereby with hydrogen (H
2) separate so that recyclable hydrogen.Described adsorbent is an active carbon, but is not limited to this, can use other any suitable adsorbents.
The hydrogen of separating can turn back in the polysilicon production process, with the trichlorosilane reaction, produce polysilicon, thereby the hydrogen in the tail gas can be recycling in polysilicon production process, reduced production cost, improved the utilization ratio of raw material.And, owing to adopt the dry method recovery technology, reduced the generation of pollutant, avoid environmental pollution, and eliminated and handled the needs of pollutant, thereby reduced production cost and energy resource consumption.
Further, the silicon tetrachloride that utilizes of the present invention also comprises hydrogen chloride (HCl) and silicon tetrachloride (SiCl to being adsorbed in the active carbon to the method that the production tail gas that polysilicon produced reclaims
4) removal process.
Particularly, at first ((here, described chlorosilane main component is silicon tetrachloride (SiCl to the hydrogen chloride (HCl) that is adsorbed in the active carbon and chlorosilane
4)) heat, be heated to temperature and be approximately 80～220 ℃, thereby the locomotor activity of raising gas molecule utilizes for example highly purified hydrogen (H then
2) (here, described chlorosilane main component is silicon tetrachloride (SiCl will to heat the back hydrogen chloride (HCl) of gaseous state and chlorosilane
4)) blow out (taking out of), need to prove that the said temperature condition only is an example, the present invention is not limited to this.And then, will be by hydrogen (H
2) gaseous hydrogen chloride (HCl) taken out of and chlorosilane and hydrogen turns back in the middle of the tail gas in the lump, the circulation of carrying out is once more reclaimed.By such process, make in the tail gas hydrogen (H as accessory substance
2) can access recovery and recycling, both can be used as the auxiliary material in the production of polysilicon reduction process, also can be used for hydrogen chloride (HCl) and chlorosilane (silicon tetrachloride (SiCl
4)) in the recycling technology of from acticarbon, taking out of, make in the process of the production of whole polysilicon and vent gas treatment, do not produce new accessory substance, make also that simultaneously original raw materials for production---activated carbon of sorbent is able to utilization sufficient, capable of circulation, and then given prominence to the effect of efficient, energy-saving and environmental protection of the present invention more.
In addition, the liquid silicon tetrachloride that has dissolved hydrogen chloride and dichloro-dihydro silicon is heated up and/or pressurizes, hydrogen chloride and dichloro-dihydro silicon are desorbed from stripping liquid;
The hydrogen chloride of the gaseous state that desorbs by control and the pressure and/or the temperature of dichloro-dihydro silicon make dichloro-dihydro silicon become liquid state, thereby separating hydrogen chloride and dichloro-dihydro silicon reclaim hydrogen chloride and/or dichloro-dihydro silicon thus.
Further, by heating up and/or pressurization, according to embodiments of the invention, the described absorbent that has dissolved hydrogen chloride and dichloro-dihydro silicon is raised to 70～220 ℃; The described absorbent that has dissolved hydrogen chloride and dichloro-dihydro silicon is pressurized to 0.1～2.0Mpa; The hydrogen chloride and the dichloro-dihydro silicon that are dissolved in the stripping liquid are desorbed.Certainly, above-mentioned pressure condition 0.1～2.0Mpa and temperature conditions only are exemplary for 70～220 ℃, as long as hydrogen chloride can be desorbed for persons of ordinary skill in the art may appreciate that, any suitable pressure and temperature condition can be used.
Then in like manner, utilize the difference of two kinds of boiling point substances, gaseous hydrogen chloride and the dichloro-dihydro silicon that is desorbed is passed through controlled pressure and/or control temperature again, carry out gas-liquid separation, more specifically, the temperature of the hydrogen chloride of the gaseous state that wherein desorbs and dichloro-dihydro silicon is controlled to be 30～-70 ℃, the pressure of the hydrogen chloride of the gaseous state that desorbs and dichloro-dihydro silicon is controlled to be 0.1～2.0Mpa, make that hydrogen chloride is gaseous state, dichloro-dihydro silicon is liquid, reclaim hydrogen chloride thus, for those having ordinary skill in the art will appreciate that, as long as gaseous hydrogen chloride and dichloro-dihydro silicon can be carried out gas-liquid separation, any suitable pressure and temperature condition can be used, therefrom with the hydrogen chloride recycle and reuse.
Certainly, above-mentioned pressure condition 0.1～2.0Mpa and temperature conditions 30～-70 ℃ only are exemplary, as long as hydrogen chloride and dichloro-dihydro silicon can be produced gas-liquid separation for persons of ordinary skill in the art may appreciate that, any suitable pressure and temperature condition can be used.
Following table shows effect that the method according to this invention and conventional wet handle the tail gas that is produced relatively in producing polysilicon.
The effect of vent gas treatment of the present invention and recovery and conventional art relatively
As can be seen, utilize method of the present invention from above-mentioned table, the rate of recovery of hydrogen, hydrogen chloride, chlorosilane and recovery quality all are much higher than traditional wet method, and purity is very high, therefore, can recycle once more, reduce consumption of raw materials, saved cost, reduced pollution.
For the ordinary skill in the art, can be to the method for utilizing silicon tetrachloride that the production tail gas that polysilicon produced is reclaimed of the present invention, carry out various conspicuous improvement, and be applied in the middle of other technologies of utilizing industrial silicon production polysilicon.
Although foregoing has illustrated and has described embodiments of the invention, but for those skilled in the art in this area, without departing from the principles and spirit of the present invention, can change these embodiment, so scope of the present invention is limited by claims and equivalent processes thereof.
Claims (10)
1, the method for utilizing silicon tetrachloride that the production tail gas that polysilicon produced is reclaimed, described tail gas mainly comprises hydrogen, hydrogen chloride and chlorosilane, described chlorosilane mainly comprises dichloro-dihydro silicon, trichlorosilane and silicon tetrachloride, said method comprising the steps of:
Silicon tetrachloride with liquid state carries out drip washing to tail gas, the impurity in the tail gas of place to go and the hydrogen chloride of absorption portion and chlorosilane;
Tail gas after the drip washing is pressurizeed and cools off, described hydrogen, hydrogen chloride, dichloro-dihydro silicon remain gaseous state, thereby separate with silicon tetrachloride with the trichlorosilane of liquid state by hydrogen, hydrogen chloride and the dichloro-dihydro silicon of gas-liquid separation with gaseous state so that make described trichlorosilane and silicon tetrachloride become liquid;
The hydrogen, hydrogen chloride and the dichloro-dihydro silicon that make gaseous state, so that the hydrogen chloride of gaseous state and dichloro-dihydro silicon are dissolved in the liquid silicon tetrachloride thereby separate with hydrogen chloride hydrogen by liquid silicon tetrachloride with dichloro-dihydro silicon;
Utilize gaseous hydrogen chloride and chlorosilane remaining in adsorbents adsorb and the filtering hydrogen, thereby hydrogen is separated with chlorosilane with the hydrogen chloride of described remnants, thus recover hydrogen;
Hydrogen chloride and the chlorosilane that is attracted in the adsorbent heated, and utilize gaseous hydrogen chloride and chlorosilane after hydrogen will heat in adsorbent, to take out of and turn back to the tail gas;
The liquid silicon tetrachloride that has dissolved hydrogen chloride and dichloro-dihydro silicon is heated up and/or pressurizes, hydrogen chloride and dichloro-dihydro silicon are desorbed from stripping liquid;
The hydrogen chloride of the gaseous state that desorbs by control and the pressure and/or the temperature of dichloro-dihydro silicon make dichloro-dihydro silicon become liquid state, thereby separating hydrogen chloride and dichloro-dihydro silicon reclaim hydrogen chloride and/or dichloro-dihydro silicon thus.
2, the method for utilizing silicon tetrachloride that the production tail gas that polysilicon produced is reclaimed according to claim 1, wherein said tail gas is pressurized to 0.1～0.9Mpa.
3, the method for utilizing silicon tetrachloride that the production tail gas that polysilicon produced is reclaimed according to claim 1, wherein the used silicon tetrachloride of tail gas drip washing is cooled to 20～-70 ℃.
4, the method for utilizing silicon tetrachloride that the production tail gas that polysilicon produced is reclaimed according to claim 1, wherein said adsorbent is an active carbon.
5, the method for utilizing silicon tetrachloride that the production tail gas that polysilicon produced is reclaimed according to claim 4, the hydrogen chloride and the chlorosilane that wherein are attracted in the adsorbent are heated to 80～220 ℃.
6, the silicon tetrachloride that utilizes according to claim 4 is to producing the method that tail gas that polysilicon produced reclaims, and wherein the gaseous hydrogen chloride that will be taken out of by hydrogen and chlorosilane turn back in the middle of the tail gas, so that the circulation recover hydrogen.
7, the method for utilizing silicon tetrachloride that the production tail gas that polysilicon produced is reclaimed according to claim 1, further comprise: to drip washing the liquid silicon tetrachloride of tail gas heat up and/or pressurize, the hydrogen chloride and the dichloro-dihydro silicon that are dissolved in the liquid silicon tetrachloride are desorbed from stripping liquid.
8, the method for utilizing silicon tetrachloride that the production tail gas that polysilicon produced is reclaimed according to claim 7, wherein the hydrogen chloride of the gaseous state that desorbs by control and the pressure and/or the temperature of dichloro-dihydro silicon make dichloro-dihydro silicon become liquid state, thereby separating hydrogen chloride and dichloro-dihydro silicon reclaim hydrogen chloride and/or dichloro-dihydro silicon thus.
9, the method for utilizing silicon tetrachloride that the production tail gas that polysilicon produced is reclaimed according to claim 8, the temperature of the hydrogen chloride of the gaseous state that wherein desorbs and dichloro-dihydro silicon is controlled to be 30～-70 ℃.
10, the method for utilizing silicon tetrachloride that the production tail gas that polysilicon produced is reclaimed according to claim 8, the pressure of the hydrogen chloride of the gaseous state that wherein desorbs and dichloro-dihydro silicon is controlled to be 0.1～2.0Mpa.
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| CN102229422A (en) * | 2011-03-30 | 2011-11-02 | 中国恩菲工程技术有限公司 | Method for recovering hydrogen chloride from tail gas generated in the production of polysilicon |
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Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5910295A (en) * | 1997-11-10 | 1999-06-08 | Memc Electronic Materials, Inc. | Closed loop process for producing polycrystalline silicon and fumed silica |
| CN1222471C (en) * | 2002-10-23 | 2005-10-12 | 同济大学 | Method of producing polysilicon with mixed source of trichloro-hydrosilicon and silicon tetrachloride |
| CN1330569C (en) * | 2005-06-16 | 2007-08-08 | 中国有色工程设计研究总院 | Process for pressure purification of silicon trichlorohydrgen and apparatus thereof |
-
2007
- 2007-07-31 CN CN2007101197445A patent/CN101357292B/en active Active
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| CN102229422B (en) * | 2011-03-30 | 2014-01-01 | 中国恩菲工程技术有限公司 | Method for recovering hydrogen chloride from tail gas generated in the production of polysilicon |
| CN102642812A (en) * | 2012-04-11 | 2012-08-22 | 中国恩菲工程技术有限公司 | System for recovering hydrogen chloride from reductive tail gas |
| CN104411636A (en) * | 2012-04-27 | 2015-03-11 | 森特瑟姆光伏美国有限公司 | Advanced off-gas recovery process and system |
| CN103172071A (en) * | 2013-03-27 | 2013-06-26 | 天津大学 | Device and method for preparing high-purity silane through disproportionation reactive distillation of trichlorosilane |
| CN103172071B (en) * | 2013-03-27 | 2015-06-03 | 天津大学 | Device and method for preparing high-purity silane through disproportionation reactive distillation of trichlorosilane |
| CN104291271A (en) * | 2014-09-28 | 2015-01-21 | 昆明冶研新材料股份有限公司 | Method and system for treating polysilicon tail gas |
| CN104555925A (en) * | 2014-11-05 | 2015-04-29 | 华文蔚 | Method for recycling tail gas in trichlorosilane production process |
| CN107648979A (en) * | 2016-07-26 | 2018-02-02 | 新特能源股份有限公司 | The method and system of tail gas in a kind of processing production of polysilicon |
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