CN102229422B - Method for recovering hydrogen chloride from tail gas generated in the production of polysilicon - Google Patents
Method for recovering hydrogen chloride from tail gas generated in the production of polysilicon Download PDFInfo
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- CN102229422B CN102229422B CN201110081212.3A CN201110081212A CN102229422B CN 102229422 B CN102229422 B CN 102229422B CN 201110081212 A CN201110081212 A CN 201110081212A CN 102229422 B CN102229422 B CN 102229422B
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Abstract
The invention discloses a method for recovering hydrogen chloride from tail gas generated in the production of polysilicon. The method comprises the following steps: (1) pressurizing and cooling the tail gas so as to separate gaseous hydrogen, hydrogen chloride and silicon dihydrogen dichloride from liquid trichlorosilane and silicon tetrachloride by gas-liquid separation; (2) allowing gaseous hydrogen, hydrogen chloride and silicon dihydrogen dichloride to pass through an absorbent so as to separate gaseous hydrogen from gaseous hydrogen chloride and silicon dihydrogen dichloride; (3) heating and/or decompressing the absorbent with dissolved hydrogen chloride and silicon dihydrogen dichloride so as to desorb hydrogen chloride and silicon dihydrogen dichloride from the absorbent; and (4) allowing desorbed gaseous hydrogen chloride and silicon dihydrogen dichloride to pass through active carbon so as to absorb and filter gaseous silicon dihydrogen dichloride, thereby recovering hydrogen chloride. According to the invention, hydrogen chloride in tail gas is recovered by a dry method and can be reused in the production of polysilicon; pollutants are reduced, the problem of environmental pollution is solved and cost is reduced.
Description
Technical field
The present invention relates to the recovery and treatment method of the tail gas of industrial production polysilicon generation, more specifically, relate to the method that reclaims hydrogenchloride the tail gas from producing the polysilicon generation.
Background technology
Polysilicon is the raw material for preparing silicon single crystal, finally for the production of unicircuit and electron device, is one of basic material that the information industry consumption is maximum, purity requirement is the highest, is also the Product and 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, there be know-how and technical characterstic separately in each company, through constantly research, exploitation, formed production technique separately, and, from national strategy angle separately, strict control techniques 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, nearly more than 20 of factories, what all adopt is traditional Siemens process, backward in technique, environmental pollution is serious, supplies consumption is large, and production cost is high, most losses of enterprise and in succession stop production or change the line of production.
The outstanding characteristics of tradition production of polysilicon technique are tail gas wet method recovery technologies, be that tail gas in reduction furnace is used water wash after preliminary separation chlorosilane, recover hydrogen, but do not reclaim hydrogenchloride, simultaneously, in the water wash process, the foreign gases such as water oxygen gas, carbonic acid gas can be polluted and prepare the hydrogen reclaimed, therefore a large amount of hydrogen reclaimed also needs again to purify, in addition, after hydrolyzing chlorosilane, also can produce large amount of sewage in lessivation, need further to process, also can cause environmental pollution and supplies consumption large.And the hydrogenchloride produced in production, fail to be fully utilized, and both wasted the energy, caused again environmental pollution.
Summary of the invention
The present invention is intended to overcome at least one above-mentioned shortcoming of the prior art.
For this reason, the object of the invention is to propose a kind of method that reclaims hydrogenchloride from the tail gas of producing the polysilicon generation, the method utilizes dry method from tail gas recycle hydrogenchloride, not only can the hydrogenchloride in tail gas be reclaimed fully, and can greatly reduce the generation of pollutent in production, while is recycling raw materials fully, reduces costs.
For achieving the above object, according to the method for hydrogenchloride that reclaims from the tail gas of producing the polysilicon generation of the embodiment of the present invention, described tail gas mainly comprises hydrogen (H
2), hydrogenchloride (HCl), dichloro-dihydro silicon (SiH
2cl
2), trichlorosilane (SiHCl
3) and silicon tetrachloride (SiCl
4), comprise the following steps: (1) pressurization and cooling described tail gas, so that described trichlorosilane and silicon tetrachloride become liquid state, described hydrogen, hydrogenchloride, dichloro-dihydro silicon remain gaseous state, thereby by gas-liquid separation, the hydrogen of gaseous state, hydrogenchloride and dichloro-dihydro silicon are separated with silicon tetrachloride with liquid trichlorosilane; (2) hydrogen, hydrogenchloride and the dichloro-dihydro silicon that make gaseous state, by absorption agent, in order to the hydrogenchloride of gaseous state and dichloro-dihydro silicon are dissolved in absorption agent, thereby separate with hydrogenchloride the hydrogen of gaseous state with dichloro-dihydro silicon; (3) absorption agent that has dissolved hydrogenchloride and dichloro-dihydro silicon is heated up and/or reduced pressure, hydrogenchloride and dichloro-dihydro silicon are desorbed from absorption agent; (4) make hydrogenchloride and dichloro-dihydro silicon by gac with absorption the dichloro-dihydro silicon of filtering gaseous state, thereby separating hydrogen chloride and dichloro-dihydro silicon reclaim hydrogenchloride thus.
Hydrogen chloride circulation recovering method from the tail gas of producing the polysilicon generation according to the embodiment of the present invention, owing to adopting the tail gas produced in the dry process production of polysilicon, overcome and eliminated the shortcoming of conventional wet recovery technology, hydrogenchloride in tail gas can be recovered utilization simultaneously, make the production means can be able to sufficient utilization, and greatly reduced generation and the quantity of pollutent in production.In addition, 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 quality product, reduce cost, made the construction and upgrading of production of polysilicon project obtain sufficient initiative.
In addition, can also there is following additional technical feature according to the method that reclaims hydrogenchloride from the tail gas of producing the polysilicon generation of the embodiment of the present invention:
According to one embodiment of present invention, the method is further comprising the steps of: (5) are heated the gac of the dichloro-dihydro silicon that adsorbed gaseous state, and utilize hydrogenchloride to blow out dichloro-dihydro silicon from gac; (6) control the temperature of the hydrogenchloride blow out and dichloro-dihydro silicon and/or pressure from activated carbon so that dichloro-dihydro silicon be liquid state and hydrogenchloride for liquid, thereby separating hydrogen chloride and dichloro-dihydro silicon.Thus, can be recycled dichloro-dihydro silicon composition wherein, further improved the utilization ratio of raw material.
Alternatively, in step (5), the gac that has adsorbed the dichloro-dihydro silicon of gaseous state can be heated to 80～180 ℃.
Alternatively, in step (6), the temperature of hydrogenchloride and dichloro-dihydro silicon is controlled as-20～-40 ℃.
According to one embodiment of present invention, the hydrogenchloride that the middle separation of step (6) is obtained returns to step (4) and is processed, and will reclaim the hydrogenchloride synthetic or chlorine hydrogenation for trichlorosilane obtained in step (4).
According to one embodiment of present invention, described tail gas is pressurizeed and cooling before with liquid silicon tetrachloride, described tail gas is carried out to drip washing, impurity absorption portion hydrogenchloride and chlorosilane with removal in tail gas.
According to one embodiment of present invention, in step (1), described tail gas is pressurized to 0.3～0.9MPa and is cooled to-20～-70 ℃.
Described absorption agent can be liquid silicon tetrachloride.
Alternatively, in step (3), the described absorption agent that has dissolved hydrogenchloride and dichloro-dihydro silicon is raised to 70～220 ℃.
The additional feature and advantage of the present invention will partly provide in the following description, and part will become obviously from the following description, or recognize by practice of the present invention.
The accompanying drawing explanation
The industrial production schematic flow sheet that Fig. 1 is polysilicon;
Fig. 2 is schematic flow sheet according to an embodiment of the invention;
Fig. 3 is schematic flow sheet in accordance with another embodiment of the present invention; With
The schematic flow sheet that Fig. 4 is another embodiment according to the present invention.
Embodiment
Describe specific embodiment in order to explain the present invention below by the reference accompanying drawing, described embodiment is exemplary, can not be interpreted as limitation of the present invention.
Fig. 1 shows the schema of industrial production polysilicon.
Have in the prior art several different methods can carry out the production of industrialization polysilicon, for example, utilizing industrial silicon and hydrogenchloride (HCl) is main raw material, by controlling reaction conditions, generates with trichlorosilane (SiHCl
3) be master's chlorosilane and the mixture of hydrogen, then pass through existing purification techniques to trichlorosilane (SiHCl
3) purified after, send into reduction furnace, make trichlorosilane (SiHCl
3) and auxiliary material hydrogen (H
2) reaction, reduction generates polysilicon.
Reaction main in production process is:
Si+HCl→SiHCl
3+SiCl
4+H
2
SiHCl
3→Si+SiCl
4+H
2
SiHCl
3+H
2→Si+HCl
In the process of above-mentioned industrial production polysilicon, the tail gas of generation comprises hydrogen (H
2), hydrogenchloride (HCl) and chlorosilane, described chlorosilane mainly comprises dichloro-dihydro silicon (SiH
2cl
2), trichlorosilane (SiHCl
3) and silicon tetrachloride (SiCl
4).
It should be noted that, owing to also having plurality of impurities in primary industry silicon, for example iron, aluminium, boron, calcium etc., so, also can produce the muriate of calcium, the muriate of iron, the muriate of aluminium and the muriate of boron in reaction, and solid and/or the gaseous impurities such as other high chlorosilanes, these impurity also can be mixed in the middle of tail gas, and content is less certainly.
Contain a large amount of hydrogen and hydrogenchloride in the tail gas that above-mentioned production polysilicon produces.To this, by the method that reclaims hydrogenchloride from produce the tail gas that polysilicon produces according to the embodiment of the present invention, hydrogenchloride is wherein reclaimed.
Embodiment 1:
Below with reference to Fig. 2, the method for hydrogenchloride that reclaims according to the embodiment of the present invention 1 is described from the tail gas of producing the polysilicon generation.
(1) pressurization and cooling above-mentioned tail gas, for example, be pressurized to about 0.3～0.9MPa by tail gas and be cooled to approximately-20～-70 ℃.Due to described trichlorosilane (SiHCl
3) and silicon tetrachloride (SiCl
4) and described hydrogen (H
2), hydrogenchloride (HCl), dichloro-dihydro silicon (SiH
2cl
2) between the boiling point difference, therefore, under above-mentioned processing condition, the trichlorosilane (SiHCl in tail gas
3) and silicon tetrachloride (SiCl
4) become liquid state, and described hydrogen (H
2) still remain gaseous state, described hydrogenchloride (HCl) and dichloro-dihydro silicon (SiH simultaneously
2cl
2) also mainly with gaseous form, exist, thereby by gas-liquid separation, just the hydrogen of gaseous state, hydrogenchloride and dichloro-dihydro silicon can be separated with silicon tetrachloride with liquid trichlorosilane.
It should be noted that, above-mentioned pressure condition 0.3～0.9MPa and temperature condition-20～-70 ℃ are only exemplary, for those having ordinary skill in the art will appreciate that, as long as can the hydrogen of gaseous state, hydrogenchloride and dichloro-dihydro silicon be separated with silicon tetrachloride with liquid trichlorosilane by gas-liquid separation, any suitable pressure and temperature condition can be used.
(2) hydrogen, hydrogenchloride and the dichloro-dihydro silicon that make gaseous state, by absorption agent, for example can utilize liquid silicon tetrachloride (SiCl
4) as absorption agent, can make hydrogenchloride (HCl) and the dichloro-dihydro silicon (SiH of gaseous state
2cl
2) be dissolved in absorption agent, thereby can be by the hydrogen (H of gaseous state
2) and hydrogenchloride (HCl) and dichloro-dihydro silicon (SiH
2cl
2) initial gross separation.
It should be noted that, absorption agent is not limited to liquid silicon tetrachloride.
In isolated gaseous hydrogen, likely contain gaseous hydrogen chloride (HCl) and the silicon tetrachloride (SiCl of a small amount of remnants
4) be mixed in wherein.To this, can utilize sorbent material 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 by hydrogen (H
2) separate.Described sorbent material is gac, but is not limited to this, can use other any suitable sorbent materials.
The hydrogen of separating can turn back in polysilicon production process, with trichlorosilane, reacts, and produces polysilicon, thereby the hydrogen in tail gas can recycle in polysilicon production process, has reduced production cost, has improved the utilising efficiency of raw material.And, owing to adopting the dry method recovery technology, reduced the generation of pollutent, avoid environmental pollution, and eliminated and processed the needs of pollutent, thereby reduced production cost and energy consumption.
(3) absorption agent that has dissolved hydrogenchloride and dichloro-dihydro silicon is heated up, for example be warming up to 70～220 ℃, hydrogenchloride and dichloro-dihydro silicon are desorbed from absorption agent.
For persons of ordinary skill in the art may appreciate that can also be by decompression (or heat up time decompression) suitably so that the hydrogenchloride and the dichloro-dihydro silicon that are dissolved in absorption agent desorb.In addition, 70～220 ℃ of said temperature conditions are only exemplary, as long as hydrogenchloride can be desorbed, any suitable pressure, temperature condition can be used.
(4) make hydrogenchloride and dichloro-dihydro silicon by gac with absorption the dichloro-dihydro silicon of filtering gaseous state, thereby separating hydrogen chloride and dichloro-dihydro silicon reclaim hydrogenchloride thus.
Although consider that hydrogenchloride is different with the boiling point of dichloro-dihydro silicon, also can so that being carried out to liquid gas, hydrogenchloride and dichloro-dihydro silicon separate by pressurization and/or cooling, yet the dividing potential drop of considering dichloro-dihydro silicon in hydrogenchloride now and dichloro-dihydro silicon mixed gas is less, want (in other words its liquefy is needed to larger cold, lower temperature and/or larger pressure), so cost is higher.In view of this, in the present embodiment, make hydrogenchloride and dichloro-dihydro silicon by gac, can make dichloro-dihydro silicon be adsorbed in gac and, by filtering, therefore according to the recovery method of the present embodiment, there is little, the easy-operating advantage of power consumption.
Thus, can be recycled the hydrogenchloride in tail gas.Particularly, as Figure 3-Figure 4, the hydrogenchloride of separating can turn back in polysilicon production process, with industrial silicon, reacts, with the synthetic or chlorine hydrogenation for trichlorosilane.Thereby the hydrogenchloride in tail gas can reduce production cost by recycle fully in polysilicon production process, has improved the utilising efficiency of raw material.And, reduced the generation of pollutent, avoid environmental pollution, and eliminated and processed the needs of pollutent, thereby reduced production cost and energy consumption.
Embodiment 2:
As shown in Figure 3, in the present embodiment, after being processed tail gas, the mode with identical with embodiment 1 further carried out following processing:
(5) gac of the dichloro-dihydro silicon that adsorbed gaseous state heated, and utilize hydrogenchloride to blow out dichloro-dihydro silicon from gac.
Particularly, at first the gac that has adsorbed hydrogenchloride (HCl) and dichloro-dihydro silicon is heated, for example can be heated to temperature and be approximately 80～180 ℃, to improve the locomotor activity of gas molecule, for example then utilize highly purified hydrogenchloride will heat hydrogenchloride (HCl) and the dichloro-dihydro silicon of gaseous state afterwards and blow out (taking out of).
(6) control the temperature of the hydrogenchloride blow out and dichloro-dihydro silicon and/or pressure from activated carbon so that dichloro-dihydro silicon be liquid state and hydrogenchloride for liquid, thereby separating hydrogen chloride and dichloro-dihydro silicon.
Particularly, make the hydrogenchloride that blows out from gac and the temperature of dichloro-dihydro silicon be for example-20～-40 ℃, due to hydrogenchloride and dichloro-dihydro silicon so that the boiling point of dichloro-dihydro silicon is different, under the said temperature condition, dichloro-dihydro silicon is liquid for liquid state hydrogenchloride, thus can separating hydrogen chloride and dichloro-dihydro silicon.It should be noted that, in mixed gas due to the hydrogenchloride blown out from gac and dichloro-dihydro silicon, hydrogenchloride is to use in order to take dichloro-dihydro silicon out of by its high pressure, therefore the dividing potential drop of hydrogenchloride is less and dividing potential drop dichloro-dihydro silicon is larger, the hydrogenchloride that can easily blow out from activated carbon by control in the case, and temperature and/or the pressure of dichloro-dihydro silicon are implemented gas-liquid separation to it.
In addition, separating obtained hydrogenchloride (wherein may contain again a small amount of dichloro-dihydro silicon) can turn back to step (4) and further processed by gac.It should be noted that, except controlling temperature, for persons of ordinary skill in the art may appreciate that suitably control pressure can be realized above-mentioned processing equally.In addition, the said temperature condition is only example, and the present invention is not limited to this, as long as hydrogenchloride and dichloro-dihydro silicon can be produced to gas-liquid separation, any suitable pressure and temperature condition can be used.
By above-mentioned processing, make the hydrogenchloride (HCl) and the dichloro-dihydro silicon that are adsorbed in gac can be recycled and recycle.Wherein, the hydrogenchloride reclaimed (HCl) can be further used for dichloro-dihydro silicon is blown out from gac, make in the process of the production of whole polysilicon and vent gas treatment, do not produce new by product, also making original raw materials for production simultaneously---the gac as sorbent material is able to utilization sufficient, capable of circulation, has therefore further strengthened efficient, energy-saving and environmental protection effect.
Embodiment 3:
As shown in Figure 4, at first, described tail gas is pressurizeed and cooling before with liquid silicon tetrachloride, tail gas is carried out to drip washing, with hydrogenchloride and the chlorosilane of the impurity in the tail gas of place to go absorption portion.
As mentioned above, described tail gas is except mainly comprising hydrogen (H
2), hydrogenchloride (HCl), dichloro-dihydro silicon (SiH
2cl
2), trichlorosilane (SiHCl
3) and silicon tetrachloride (SiCl
4), in the process of producing polysilicon, also can produce the impurity such as the solid impurity such as the muriate of calcium, the muriate of iron, the muriate of aluminium and the muriate of boron and high chlorosilane, therefore, utilize liquid silicon tetrachloride (SiCl
4) tail gas is carried out to drip washing not only can remove the above-mentioned impurity in tail gas, and can avoid causing the hydrolysis of chlorosilane.In summary, according to embodiments of the invention, lessivation adopts liquid silicon tetrachloride (SiCl
4), the effect that carries out drip washing with traditional water is not identical.
In addition, owing in the production reduction process at polysilicon, also can producing by product---silicon tetrachloride (SiCl
4), common every production 1kg polysilicon can produce the silicon tetrachloride (SiCl of 10kg left and right
4).According to the present invention, can be by the silicon tetrachloride that produces in production of polysilicon for tail gas is carried out to drip washing, thus can make material obtain recycle in production of polysilicon.
After this, in the mode identical with embodiment 2, tail gas is processed.
Utilize method and the conventional wet of embodiment 3 to recycle the hydrogenchloride contained in the tail gas of producing the polysilicon generation, the results are shown in table 1.
Table 1
As can be seen from Table 1, utilize method of the present invention, the rate of recovery of hydrogenchloride and recovery quality are all far away higher than traditional wet method, according to the present invention, hydrogenchloride almost completely be recycled and purity very high, therefore, can be as react and produce the raw material of polysilicon with industrial silicon, thus recycled, reduced the consumption of raw material, saved cost, reduced pollution, and effect is apparent from above table.
For the ordinary skill in the art, can, to the method that reclaims hydrogenchloride from the tail gas of producing the polysilicon generation of the present invention, carry out various apparent improvement, and be applied in the middle of other techniques of utilizing the industrial silicon production polysilicon.
Although foregoing has illustrated and has described embodiments of the invention, but for those ordinary skill in the art, without departing from the principles and spirit of the present invention, can be changed these embodiment, therefore scope of the present invention is limited by claims and equivalent processes thereof.
Claims (9)
1. reclaim the method for hydrogenchloride from the tail gas of producing the polysilicon generation, described tail gas mainly comprises hydrogen, hydrogenchloride and chlorosilane, and described chlorosilane comprises dichloro-dihydro silicon, trichlorosilane and silicon tetrachloride, said method comprising the steps of:
(1) pressurization and cooling described tail gas, so that described trichlorosilane and silicon tetrachloride become liquid state, described hydrogen, hydrogenchloride, dichloro-dihydro silicon remain gaseous state, thereby by gas-liquid separation, the hydrogen of gaseous state, hydrogenchloride and dichloro-dihydro silicon are separated with silicon tetrachloride with liquid trichlorosilane;
(2) hydrogen, hydrogenchloride and the dichloro-dihydro silicon that makes gaseous state is by absorption agent, so that the hydrogenchloride of gaseous state and dichloro-dihydro silicon is dissolved in absorption agent, thereby the hydrogen of gaseous state separated with dichloro-dihydro silicon with hydrogenchloride;
(3) absorption agent that has dissolved hydrogenchloride and dichloro-dihydro silicon is heated up and/or reduced pressure, hydrogenchloride and dichloro-dihydro silicon are desorbed from absorption agent; With
(4) make hydrogenchloride and dichloro-dihydro silicon by gac with absorption the dichloro-dihydro silicon of filtering gaseous state, thereby separating hydrogen chloride and dichloro-dihydro silicon reclaim hydrogenchloride thus.
2. reclaim the method for hydrogenchloride the tail gas produced from the production polysilicon according to claim 1, further comprising the steps of:
(5) gac of the dichloro-dihydro silicon that adsorbed gaseous state heated, and utilize hydrogenchloride to blow out dichloro-dihydro silicon from gac; With
(6) control the temperature of the hydrogenchloride blow out and dichloro-dihydro silicon and/or pressure from activated carbon so that dichloro-dihydro silicon be liquid state and hydrogenchloride for liquid, thereby separating hydrogen chloride and dichloro-dihydro silicon.
3. the method that reclaims hydrogenchloride from produce the tail gas that polysilicon produces according to claim 2, in step (5), will adsorb the heating activated carbon to 80 of the dichloro-dihydro silicon of gaseous state～180 ℃.
4. the method that reclaims hydrogenchloride from the tail gas of producing the polysilicon generation according to claim 2, in step (6), control the temperature of hydrogenchloride and dichloro-dihydro silicon for-20～-40 ℃.
5. reclaim the method for hydrogenchloride the tail gas produced from the production polysilicon according to claim 2, the hydrogenchloride that the middle separation of step (6) is obtained returns to step (4) and is processed, and will reclaim the hydrogenchloride synthetic or chlorine hydrogenation for trichlorosilane obtained in step (4).
6. reclaim the method for hydrogenchloride the tail gas produced from the production polysilicon according to claim 1, wherein, described tail gas is pressurizeed and cooling before with liquid silicon tetrachloride, described tail gas is carried out to drip washing, impurity absorption portion hydrogenchloride and chlorosilane with removal in tail gas.
7. reclaim the method for hydrogenchloride the tail gas produced from the production polysilicon according to claim 1, in step (1), described tail gas is pressurized to 0.3～0.9MPa and is cooled to-20～-70 ℃.
8. reclaim the method for hydrogenchloride the tail gas produced from the production polysilicon according to claim 1, wherein said absorption agent is liquid silicon tetrachloride.
9. reclaim the method for hydrogenchloride the tail gas produced from the production polysilicon according to claim 4, in step (3), the described absorption agent that has dissolved hydrogenchloride and dichloro-dihydro silicon is raised to 70～220 ℃.
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| CN101357292A (en) * | 2007-07-31 | 2009-02-04 | 中国恩菲工程技术有限公司 | Method for recovering tail-gas generated during producing polycrystalline silicon using silicon tetrachloride |
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| CN101357292A (en) * | 2007-07-31 | 2009-02-04 | 中国恩菲工程技术有限公司 | Method for recovering tail-gas generated during producing polycrystalline silicon using silicon tetrachloride |
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| Title |
|---|
| 环氧氯丙烷生产技术和发展意见;薛祖源;《中国氯碱》;20070630(第6期);第40页右侧栏第2段 * |
| 薛祖源.环氧氯丙烷生产技术和发展意见.《中国氯碱》.2007,(第6期),第40页右侧栏第2段. |
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