CN101357287B - Method for recovering hydrogen chloride from off-gas generated from the production of polycrystalline silicon - Google Patents
Method for recovering hydrogen chloride from off-gas generated from the production of polycrystalline silicon Download PDFInfo
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- CN101357287B CN101357287B CN200710119745XA CN200710119745A CN101357287B CN 101357287 B CN101357287 B CN 101357287B CN 200710119745X A CN200710119745X A CN 200710119745XA CN 200710119745 A CN200710119745 A CN 200710119745A CN 101357287 B CN101357287 B CN 101357287B
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Abstract
A method for recovering hydrogen chloride from tail gas generated from polysilicon production comprises the following steps: the tail gas is leached at low temperature, pressurized and cooled for gas-liquid separation; gaseous hydrogen, hydrogen chloride and the dichlordihydrosilicate pass through a liquid absorbent to cause the gaseous hydrogen chloride and the dichlordihydrosilicate to be dissolved in the liquid absorbent, and the hydrogen is separated from the hydrogen chloride and the dichlordihydrosilicate; the hydrogen chloride and the dichlordihydrosilicate dissolved in the liquid absorbent are desorbed by increasing the temperature; the gas-liquid separation is carried out on the desorbed gaseous hydrogen chloride and the dichlordihydrosilicate by controlling the pressure and/or the temperature, therefore, the hydrogen chloride becomes gaseous and the dichlordihydrosilicate becomes liquid, and then the hydrogen chloride is recovered. By adopting dry processing, the hydrogen chloride is recovered from the tail gas and 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 commercial production polysilicon produced, more specifically, relate to a kind of method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride.
Background technology
Polysilicon is the raw material of preparation monocrystalline silicon, finally is used to produce integrated circuit and electronic device, is one of basic material that the information industry consumption is maximum, purity requirement is the highest, also is the product and the industry of state key encourage growth.
The advanced production of polysilicon technology in the world 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, and middle nineteen sixties is realized industrialization, and 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, and production cost is high, 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, and promptly the tail gas in the reduction furnace is used water wash, recover hydrogen after preliminary pressurization separates chlorosilane; But do not reclaim hydrogen chloride, simultaneously, because in the water wash process; Foreign gases such as water oxygen gas, carbon dioxide can be polluted the hydrogen of preparing recovery, so the hydrogen of recovery also needs to purify once more in a large number, in addition; In the lessivation after the chlorosilane hydrolysis; Also can produce large amount of sewage, need further to handle, also can cause environmental pollution and supplies consumption big.And the hydrogen chloride that produces in the production fails to be fully utilized, and has both wasted the energy, has caused environmental pollution again.
Summary of the invention
The object of the invention is intended to overcome at least one above-mentioned shortcoming of the prior art, proposes a kind of method that can from produce the tail gas that polysilicon produced, reclaim hydrogen chloride.
Utilize method of the present invention, not only can reclaim fully and recycle, and can significantly reduce the generation of pollutant in the production, made full use of material simultaneously, reduced cost the hydrogen chloride in the tail gas.
For realizing above-mentioned purpose, embodiments of the invention propose a kind of method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride, and said tail gas mainly comprises hydrogen (H
2), hydrogen chloride (HCl), dichloro-dihydro silicon (SiH
2Cl
2), trichlorosilane (SiHCl
3) and silicon tetrachloride (SiCl
4); Said method comprising the steps of: pressurize and cool off said tail gas; Said hydrogen, hydrogen chloride, dichloro-dihydro silicon remain gaseous state, thereby separate with silicon tetrachloride with the trichlorosilane of liquid state through hydrogen, hydrogen chloride and the dichloro-dihydro silicon of gas-liquid separation with gaseous state so that make said 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 absorbent thereby separate with hydrogen chloride hydrogen through liquid absorbent with dichloro-dihydro silicon; Absorbent to having dissolved hydrogen chloride and dichloro-dihydro silicon heats up and/or pressurizes, and hydrogen chloride and dichloro-dihydro silicon are desorbed from stripping liquid; The hydrogen chloride of the gaseous state that desorbs through 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 thus.
The further embodiment according to the present invention, said tail gas is pressurized to 0.3～0.9Mpa.Said tail gas is cooled to-20～-70 ℃.Said absorbent is a silicon tetrachloride.
The further embodiment according to the present invention, the method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride also comprises: the liquid silicon tetrachloride that has absorbed hydrogen chloride is heated up and/or pressurizes, make that hydrogen chloride is desorbed.
Particularly, the said liquid silicon tetrachloride that has absorbed hydrogen chloride is raised to 70～220 ℃; The said liquid silicon tetrachloride that has absorbed hydrogen chloride is pressurized to 0.1～2.0Mpa.The temperature of the hydrogen chloride of the gaseous state that 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.
Based on the further embodiment of the present invention, the described method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride also is included in before tail gas pressurization and the cooling, with liquid silicon tetrachloride tail gas is carried out drip washing.
The further embodiment according to the present invention; The method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride also comprises: the liquid silicon tetrachloride that in lessivation, has absorbed hydrogen chloride is heated up and/or pressurizes, make hydrogen chloride from liquid silicon tetrachloride, desorbed.
Particularly, the said liquid silicon tetrachloride that has absorbed hydrogen chloride is raised to 70～220 ℃.The said liquid silicon tetrachloride that has absorbed hydrogen chloride is pressurized to 0.1～2.0Mpa.
Overcome and eliminated the shortcoming of conventional wet recovery technology according to the present invention; Hydrogen chloride in the tail gas is recycled simultaneously; Especially the hydrogen chloride that reclaims 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 greatly reduces the consumption of raw and auxiliary material in closed cycle is used; 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 through practice of the present invention.
Description of drawings
Fig. 1 is the commercial production schematic flow sheet of polysilicon;
Fig. 2 is the schematic flow sheet according to first embodiment of the invention;
Fig. 3 is the schematic flow sheet according to second embodiment of the invention.
The specific embodiment
Below through describing concrete embodiment with reference to accompanying drawing so that explain the present invention, described embodiment is exemplary, can not be interpreted as limitation of the present invention.
Embodiment 1:
With reference to figure 1; Wherein show the FB(flow block) that to use according to the commercial production polysilicon of the hydrogen chloride recovery method of the embodiment of the invention; In the prior art, there is several different methods can carry out the production of industrialization polysilicon, uses 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 through 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 commercial production polysilicon, the tail gas of generation mainly comprises hydrogen (H
2), hydrogen chloride (HCl) and chlorosilane, said chlorosilane mainly comprises dichloro-dihydro silicon (SiH
2Cl
2), trichlorosilane (SiHCl
3) and silicon tetrachloride (SiCl
4).
Reaction main in the production process is:
Need to prove, owing in primary industry silicon, also have plurality of impurities, for example iron, aluminium, calcium, boron, phosphorus 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, also can handle these impurity according to the method for the invention, and this will describe below.
Describe the method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride according to first embodiment of the invention below with reference to Fig. 2, Fig. 2 shows the flow chart that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride.
At first, the tail gas that in the polysilicon production process, produces is collected, and the tail gas of collecting is pressurizeed and cools off, and for example, tail gas is pressurized to about 0.3～0.9Mpa and is cooled to approximately-20～-70 ℃, because said trichlorosilane (SiHCl
3) and silicon tetrachloride (SiCl
4) and said hydrogen (H
2), hydrogen chloride (HCl), dichloro-dihydro silicon (SiH
2Cl
2) between boiling point different, therefore, under above-mentioned process conditions, the trichlorosilane (SiHCl in the tail gas
3) and silicon tetrachloride (SiCl
4) become liquid state, and said hydrogen (H
2) still remain gaseous state, said hydrogen chloride (HCl) and dichloro-dihydro silicon (SiH simultaneously
2Cl
2) also mainly exist with gaseous form, thereby just can hydrogen, hydrogen chloride and the dichloro-dihydro silicon of gaseous state be separated with silicon tetrachloride with the trichlorosilane of liquid state through 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 through 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 most gaseous hydrogen chloride (HCl) and dichloro-dihydro silicon (SiH
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.
For the hydrogen chloride that is absorbed as absorbent by liquid silicon tetrachloride, can the hydrogen chloride and the dichloro-dihydro silicon that be dissolved in the stripping liquid be desorbed through the method that heats up and/or pressurize; In the present embodiment, it is 70～220 ℃ that employing is warmed up to, and is pressurized to 0.1～2.0Mpa simultaneously, just can hydrogen chloride and dichloro-dihydro silicon be desorbed.
Certainly; Above-mentioned pressure condition 0.1～2.0Mpa and temperature conditions only are exemplary for 70～220 ℃; As long as can hydrogen chloride and dichloro-dihydro silicon be desorbed for persons of ordinary skill in the art may appreciate that, any suitable pressure and temperature condition can be used.
In like manner; Utilize the difference of physics boiling point once more; Gaseous hydrogen chloride and dichloro-dihydro silicon to being desorbed pass through controlled pressure and/or control temperature again, carry out gas-liquid separation, make that hydrogen chloride is gaseous state; Dichloro-dihydro silicon is liquid, and collects with surge tank respectively or directly fail through pipeline and reclaim hydrogen chloride and dichloro-dihydro silicon.
The hydrogen chloride of separating can turn back in the polysilicon production process; With industrial silicon reaction, synthesizing trichlorosilane, thereby the hydrogen chloride in the tail gas can be by recycle fully in polysilicon production process; Reduce production cost, improved the utilization ratio of raw material.And, reduced the generation of pollutant, avoid environmental pollution, and eliminated and handled the needs of pollutant, thereby reduced production cost and energy resource consumption.
Embodiment 2:
Below with reference to Fig. 3 the method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride according to second embodiment of the invention is described.Fig. 3 shows the FB(flow block) according to second embodiment of the invention, and the main distinction of present embodiment and above-mentioned first embodiment is, also comprises with liquid silicon tetrachloride (SiCl
4) step of tail gas being carried out drip washing.
In the middle of traditional wet tail gas treatment process process, all be that water carries out drip washing to tail gas usually, purpose is that the hydrogen chloride (HCl) in the tail gas is got 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 individual processing, causes supplies consumption big, and environmental pollution is serious; Simultaneously also waste the hydrogen chloride that can be used as raw materials for production in a large number, 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 the impurity in the tail gas, as stated, said 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.
Simultaneously, in the present embodiment, the liquid silicon tetrachloride that in lessivation, has absorbed hydrogen chloride is heated up and/or pressurizes, make that hydrogen chloride is desorbed once more.In the present embodiment, can adopt to be warmed up to 70～220 ℃, be pressurized to 0.1～2.0Mpa simultaneously, hydrogen chloride is desorbed.And then, hydrogen chloride and the chlorosilane that is desorbed are simultaneously carried out separation and purification once more through the gas-liquid separation process.Particularly, the hydrogen chloride of the gaseous state that desorbs of said control and the temperature of dichloro-dihydro silicon are 30～-70 ℃.The pressure of the hydrogen chloride of the gaseous state that said control desorbs and dichloro-dihydro silicon is 0.1～2.0Mpa.
Certainly, 70～220 ℃ of above-mentioned pressure condition 0.1～2.0Mpa and temperature conditions, and temperature conditions 30～-70 ℃; Only be exemplary; As long as can hydrogen chloride be desorbed for persons of ordinary skill in the art may appreciate that, any suitable pressure and temperature condition can be used.
Following table shows according to the method for the invention and with conventional wet side the effect that hydrogen chloride reclaims is compared.
The present invention is to the comparison to the hydrogen chloride recovering effect of hydrogen chloride recovering effect and conventional art
| Project | The present invention | Conventional wet |
| Hydrogen chloride rate of recovery % | More than 99.99% | All drench in the entry |
| Hydrogen chloride reclaims purity | More than 99%, contain micro-chlorosilane | All drip washing entry, generation large amount of sewage |
From above-mentioned table, can find out, utilize method of the present invention, the recovery of hydrogen chloride rate all is higher than traditional wet far away with the recovery quality; According to the present invention, hydrogen chloride almost completely obtain reclaiming and purity very high, therefore; Can conduct react and produce the raw material of polysilicon, thereby recycled, reduce consumption of raw materials with industrial silicon; Practiced thrift cost, reduced pollution, and effect is obvious from above table.
For those of ordinary skill in the art, can carry out various conspicuous improvement to the method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride of the present invention, 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; Under the situation that does not break away from principle of the present invention and spirit; Can change these embodiment, so scope of the present invention is limited accompanying claims and equivalent thereof.
Claims (12)
1. method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride, said tail gas mainly comprises hydrogen, hydrogen chloride and chlorosilane, said chlorosilane mainly comprises dichloro-dihydro silicon, trichlorosilane and silicon tetrachloride, said method comprising the steps of:
Pressurization and cool off said tail gas; Said hydrogen, hydrogen chloride, dichloro-dihydro silicon remain gaseous state, thereby separate with silicon tetrachloride with the trichlorosilane of liquid state through hydrogen, hydrogen chloride and the dichloro-dihydro silicon of gas-liquid separation with gaseous state so that make said 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 absorbent thereby separate with hydrogen chloride hydrogen through liquid absorbent with dichloro-dihydro silicon;
Absorbent to having dissolved hydrogen chloride and dichloro-dihydro silicon heats up and/or pressurizes, and hydrogen chloride and dichloro-dihydro silicon are desorbed from stripping liquid;
The hydrogen chloride of the gaseous state that desorbs through 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 thus.
2. the method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride according to claim 1, wherein said tail gas is pressurized to 0.3～0.9Mpa.
3. the method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride according to claim 1, wherein said tail gas is cooled to-20～-70 ℃.
4. the method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride according to claim 1, wherein said stripping liquid is a silicon tetrachloride.
5. the method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride according to claim 1, the wherein said absorbent that has dissolved hydrogen chloride and dichloro-dihydro silicon is raised to 70～220 ℃.
6. the method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride according to claim 1, the wherein said absorbent that has dissolved hydrogen chloride and dichloro-dihydro silicon is pressurized to 0.1～2.0Mpa.
7. based on any described method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride in the claim 1～6, further comprise: before to tail gas pressurization and cooling, tail gas is carried out drip washing with liquid silicon tetrachloride.
8. the method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride according to claim 7; Wherein the liquid silicon tetrachloride that in lessivation, has absorbed hydrogen chloride is heated up and/or pressurizes, make hydrogen chloride from liquid silicon tetrachloride, desorbed.
9. the method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride according to claim 8, the wherein said liquid silicon tetrachloride that has absorbed hydrogen chloride is raised to 70～220 ℃.
10. the method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride according to claim 8, the wherein said liquid silicon tetrachloride that has absorbed hydrogen chloride is pressurized to 0.1～2.0Mpa.
11. the method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride according to claim 1, 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.
12. the method that from produce the tail gas that polysilicon produced, reclaims hydrogen chloride according to claim 1, the temperature of the hydrogen chloride of the gaseous state that wherein desorbs and dichloro-dihydro silicon is controlled to be-70 ℃～30 ℃.
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| CN200710119745XA CN101357287B (en) | 2007-07-31 | 2007-07-31 | Method for recovering hydrogen chloride from off-gas generated from the production of polycrystalline silicon |
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| CN101357287B true CN101357287B (en) | 2012-07-04 |
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| CN109843800B (en) * | 2016-10-12 | 2022-06-07 | 株式会社德山 | Method for manufacturing polycrystalline silicon |
| CN112391677B (en) * | 2020-11-12 | 2021-12-03 | 内蒙古科思通科技有限公司 | A balanced pressure reaction unit for preparation of high-purity silicon crystal |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1433958A (en) * | 2002-01-25 | 2003-08-06 | 黑龙江齐化化工有限责任公司 | Process for purifying hydrogen chloride |
| RU2274602C1 (en) * | 2004-08-16 | 2006-04-20 | Федеральное государственное унитарное предприятие "Государственный научно-исследовательский и проектный институт редкометаллической промышленности "Гиредмет" | Trichlorosilane production process |
-
2007
- 2007-07-31 CN CN200710119745XA patent/CN101357287B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1433958A (en) * | 2002-01-25 | 2003-08-06 | 黑龙江齐化化工有限责任公司 | Process for purifying hydrogen chloride |
| RU2274602C1 (en) * | 2004-08-16 | 2006-04-20 | Федеральное государственное унитарное предприятие "Государственный научно-исследовательский и проектный институт редкометаллической промышленности "Гиредмет" | Trichlorosilane production process |
Non-Patent Citations (1)
| Title |
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| 刘建军.多晶硅生产中回收氢气的净化.《有色冶炼》.2000,第29卷(第6期),第17-19页. * |
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